Chapter 10: Halogen Derivatives

In the late 1920s, a refrigerator was a dangerous thing to own. The machines were cooled by gases such as ammonia, sulphur dioxide and methyl chloride, and a cracked pipe in the night could poison an entire household. Thomas Midgley Jr., a chemist working with General Motors, was given a clear brief: design a cooling gas that will not burn and will not poison. He turned to the halogens. Starting from methane and replacing its hydrogen atoms with chlorine and fluorine, he arrived at dichlorodifluoromethane — the compound the world soon knew as Freon-12. It was odourless, non-flammable and remarkably unreactive, and Midgley is said to have demonstrated its safety before an audience of chemists by breathing it in. Within a few decades, chlorofluorocarbons were cooling homes, pushing paint out of spray cans and blowing bubbles into plastic foam.

That same unreactivity turned out to be the trouble. Nothing at ground level destroyed these molecules, so they drifted slowly upward into the stratosphere. In 1974, Mario Molina and F. Sherwood Rowland argued that ultraviolet radiation up there snaps the carbon–chlorine bond and sets free chlorine atoms, and that a single chlorine atom can go on to destroy an enormous number of ozone molecules. Their work led to the Montreal Protocol and, in 1995, to a Nobel Prize in Chemistry.

One bond, and one choice of halogen, altered the atmosphere of a planet. The picture in Fig. 10.0 shows how a molecule designed for a kitchen ended up in the sky.

Diagram

Fig. 10.0 – A CFC molecule (CCl₂F₂) rising from a refrigerator/aerosol can at ground level into the stratosphere, where a UV photon breaks the C–Cl bond to release a Cl atom that attacks an O₃ molecule; label C–Cl bond, UV radiation, ozone layer.

NoteCuriosity Corner

Q1. A CFC molecule contains both C–Cl and C–F bonds. Why does sunlight break the carbon–chlorine bond and leave the carbon–fluorine bond alone? Q2. Alkyl halides are polar molecules, and water is a polar solvent. Why, then, does an alkyl halide refuse to dissolve in water and settle as a separate layer instead? Q3. Chloroethane and chlorobenzene both contain a carbon–chlorine bond, yet a nucleophile attacks one easily and the other only under fierce conditions. What makes the ring change the bond so much? Q4. Your left hand will not fit into a right-hand glove. What does this everyday fact have to do with the way a molecule of 2-chlorobutane behaves towards a beam of light? Q5. Two alkyl halides are treated with hydroxide ion. For one of them, the rate depends on how concentrated the hydroxide is; for the other, it does not matter at all. How can the same kind of reaction behave in two such different ways?

Keep these questions with you as you read — this chapter will give you everything you need to reason out each one.

10.1 Classification of Halogen Derivatives

Identify the functional group in the following compounds. i. Benzyl bromide, \(\mathrm{C_6H_5\!-\!CH_2\!-\!Br}\) ii. Freon-12, \(\mathrm{CCl_2F_2}\) iii. Hexachlorobenzene, \(\mathrm{C_6Cl_6}\) iv. Westrosol, \(\mathrm{Cl\!-\!CH{=}CCl_2}\) v. Hexachlorocyclohexane (benzene hexachloride), \(\mathrm{C_6H_6Cl_6}\)

The structures of these five compounds are drawn together in Fig. 10.7; look carefully at which carbon atom carries the halogen in each one, because that single detail is what this section is about.

Diagram

Fig. 10.7 – Structures of benzyl bromide (benzene ring with –CH₂Br), Freon-12 (CCl₂F₂), hexachlorobenzene (benzene ring with Cl on all six carbons), Westrosol (Cl–CH=CCl₂) and hexachlorocyclohexane (cyclohexane ring with one Cl on each carbon); label the halogen atoms in each.

The parent family of all organic compounds is the hydrocarbons — molecules built from carbon and hydrogen alone. Take any hydrocarbon, whether it is aliphatic (an open chain, such as ethane) or aromatic (a benzene-type ring), and replace one or more of its hydrogen atoms by halogen atoms. What you obtain is a new family of compounds: the halogen derivatives of hydrocarbons.

A halogen is any member of Group 17 of the periodic table — fluorine, chlorine, bromine or iodine. Since all four behave in a broadly similar way here, chemists use the general symbol \(\mathrm{X}\) to stand for any one of them and write a halogen derivative compactly as \(\mathrm{R\!-\!X}\), where \(\mathrm{R}\) is the hydrocarbon part of the molecule.

NoteDefinition

A halogen derivative of a hydrocarbon is a compound formed when one or more hydrogen atoms of an aliphatic or aromatic hydrocarbon are replaced by halogen atoms.

This replacement does far more than swap one small atom for another. A halogen is much more electronegative than carbon, so the new \(\mathrm{C\!-\!X}\) bond is polar, and that polarity turns an otherwise unreactive hydrocarbon into a molecule with a definite reactive site. This is why the halogen derivatives are so useful as starting materials for making alcohols, ethers, amines, nitriles and a great many other compounds. In this chapter we will study them in a systematic way.

Halogen derivatives are classified mainly in two ways.

Classification by the Carbon Skeleton

The first scheme looks at the kind of hydrocarbon skeleton to which the halogen atom is bonded. On this basis, halogen derivatives are classified as haloalkanes, haloalkenes, haloalkynes and haloarenes, as shown in Fig. 10.8.

\[\mathrm{CH_3\!-\!CH_2\!-\!X}\ \text{(haloalkane)} \qquad \mathrm{CH_2{=}CH\!-\!X}\ \text{(haloalkene)}\]

\[\mathrm{HC{\equiv}C\!-\!X}\ \text{(haloalkyne)} \qquad \mathrm{C_6H_5\!-\!X}\ \text{(haloarene)}\]

Diagram

Fig. 10.8 – Four general structures side by side: CH₃–CH₂–X labelled haloalkane, CH₂=CH–X labelled haloalkene, HC≡C–X labelled haloalkyne, and a benzene ring bearing X labelled haloarene.

The naming pattern is easy to read: the prefix halo- is simply attached to the name of the parent skeleton — alkane, alkene, alkyne or arene.

Classification by the Number of Halogen Atoms

The second scheme simply counts how many halogen atoms the molecule carries. On this basis, halogen derivatives are classified as mono, di, tri or poly halogen compounds. Representative structures are given in Fig. 10.9.

A monohalogen compound carries exactly one halogen atom, as in \(\mathrm{CH_3\!-\!CH_2\!-\!X}\) or \(\mathrm{C_6H_5\!-\!X}\). A dihalogen compound carries two, as in \(\mathrm{CH_3\!-\!CHX_2}\), in \(\mathrm{CH_2X\!-\!CH_2X}\), or in an ortho-dihalobenzene. A trihalogen compound carries three, as in \(\mathrm{CH_2X\!-\!CHX\!-\!CH_2X}\) or in a trihalobenzene.

Diagram

Fig. 10.9 – Three rows of examples: (row 1, monohalogen) CH₃–CH₂–X and benzene ring with one X; (row 2, dihalogen) CH₃–CHX₂, CH₂X–CH₂X and benzene ring with two X at adjacent positions; (row 3, trihalogen) CH₂X–CHX–CH₂X and benzene ring with three X at alternate positions.

Two dihalogen compounds may carry their halogens very differently. When both halogen atoms sit on the same carbon, as in \(\mathrm{CH_3\!-\!CHX_2}\), the compound is called a geminal dihalide; when they sit on adjacent carbons, as in \(\mathrm{CH_2X\!-\!CH_2X}\), it is called a vicinal dihalide. You will meet the vicinal dihalides again when alkenes add chlorine or bromine.

We will now consider the classification of monohalogen derivatives in more detail. The complete classification scheme is collected in FC 10.1.

Flowchart

FC 10.1 – Classification of halogen derivatives: halogen derivatives of hydrocarbons → branch A (basis: carbon skeleton) → haloalkanes / haloalkenes / haloalkynes / haloarenes; → branch B (basis: number of halogen atoms) → mono / di / tri / poly halogen compounds; mono halogen compounds → (basis: position of X and hybridization of C) → alkyl halide → further branch: primary (1°) / secondary (2°) / tertiary (3°); allylic halide; benzylic halide; vinylic halide; haloalkyne; aryl halide.

Q. Allyl chloride, \(\mathrm{CH_2{=}CH\!-\!CH_2\!-\!Cl}\), contains a carbon–carbon double bond. Should it then be called a haloalkene?

A. No. What decides the class is the carbon that actually carries the halogen. In allyl chloride the chlorine sits on a saturated \(\mathrm{sp^3}\) carbon, so the molecule behaves as an alkyl-type halide; the double bond is present elsewhere in the chain. In a true haloalkene such as vinyl chloride, \(\mathrm{CH_2{=}CH\!-\!Cl}\), the halogen is bonded to the doubly bonded carbon itself.

The word halogen comes from the Greek hals, meaning salt, and genes, meaning forming — literally “salt former”, a name given to these elements because they combine with metals to give common salts such as sodium chloride. The prefix allyl has an equally direct origin: the first allyl compounds were obtained from the pungent oil of garlic, whose botanical name is Allium sativum.

10.1.1 Classification of Monohalogen Compounds

Monohalogen compounds are classified further on the basis of two things: the position of the halogen atom in the molecule, and the type of hybridization of the carbon atom to which the halogen is attached.

Alkyl Halides or Haloalkanes

In alkyl halides, also called haloalkanes, the halogen atom is bonded to an \(\mathrm{sp^3}\) hybridized carbon which is part of a saturated carbon skeleton.

Alkyl halides are further described as primary, secondary or tertiary, depending on the substitution state of the carbon that carries the halogen — that is, on how many other carbon atoms are directly attached to it (refer to Std. XI Chemistry Textbook, section 14.3). If that carbon is joined to one carbon it is primary, to two carbons secondary, and to three carbons tertiary. These three types are drawn in Fig. 10.10.

\[\mathrm{R\!-\!CH_2\!-\!X}\ \text{(primary, 1}^\circ\text{)} \qquad \mathrm{R\!-\!CHX\!-\!R}\ \text{(secondary, 2}^\circ\text{)} \qquad \mathrm{R_3C\!-\!X}\ \text{(tertiary, 3}^\circ\text{)}\]

Diagram

Fig. 10.10 – Three structures with the halogen-bearing carbon highlighted: R–CH₂–X labelled primary halide (1° halide), R–CHX–R labelled secondary halide (2° halide), and R–C(R)(R)–X labelled tertiary halide (3° halide).

This 1°/2°/3° label is worth learning properly now. It will decide, later in this chapter, which mechanism an alkyl halide follows when a nucleophile attacks it.

Allylic Halides

In allylic halides, the halogen atom is bonded to an \(\mathrm{sp^3}\) hybridized carbon atom that lies next to a carbon–carbon double bond.

\[\mathrm{CH_2{=}CH\!-\!CH_2\!-\!X}\]

A cyclic example is 3-halocyclohexene, in which the halogen sits on the saturated carbon immediately next to the ring double bond.

Benzylic Halides

In benzylic halides, the halogen atom is bonded to an \(\mathrm{sp^3}\) hybridized carbon atom which is itself further bonded to an aromatic ring.

\[\mathrm{C_6H_5\!-\!CH_2\!-\!X} \qquad \mathrm{C_6H_5\!-\!C(CH_3)_2\!-\!X}\]

Notice the difference from an aryl halide: here the halogen is one carbon away from the ring, not on it.

Vinylic Halides

In vinylic halides, the halogen atom is bonded to an \(\mathrm{sp^2}\) hybridized carbon atom of an aliphatic chain. A vinylic halide is therefore a haloalkene.

\[\mathrm{CH_2{=}CH\!-\!X}\]

A halogen placed directly on the doubly bonded carbon of a cyclohexene ring gives a cyclic vinylic halide.

Haloalkynes

When a halogen atom is bonded to an \(\mathrm{sp}\) hybridized carbon atom, the compound is a haloalkyne.

\[\mathrm{CH{\equiv}C\!-\!X}\]

Aryl Halides or Haloarenes

In aryl halides, the halogen atom is directly bonded to an \(\mathrm{sp^2}\) hybridized carbon atom of an aromatic ring.

\[\mathrm{C_6H_5\!-\!X}\]

An example carrying a substituent as well is o-halotoluene, in which a methyl group occupies the position next to the halogen. All six classes are drawn together in Fig. 10.11.

Diagram

Fig. 10.11 – Six labelled structures in one panel with the hybridization of the halogen-bearing carbon marked below each: alkyl halide (R–CH₂–X, sp³), allylic halide (CH₂=CH–CH₂–X, sp³), benzylic halide (C₆H₅–CH₂–X, sp³), vinylic halide (CH₂=CH–X, sp²), haloalkyne (CH≡C–X, sp), aryl halide (benzene ring with X, sp²).

alkyl vs allylic vs benzylic vs vinylic vs haloalkyne vs aryl halides

Class Where the halogen sits Hybridization of that carbon Example
Alkyl halide (haloalkane) On a saturated carbon of the chain \(\mathrm{sp^3}\) \(\mathrm{CH_3\!-\!CH_2\!-\!X}\)
Allylic halide On a saturated carbon next to a C=C \(\mathrm{sp^3}\) \(\mathrm{CH_2{=}CH\!-\!CH_2\!-\!X}\)
Benzylic halide On a saturated carbon attached to an aromatic ring \(\mathrm{sp^3}\) \(\mathrm{C_6H_5\!-\!CH_2\!-\!X}\)
Vinylic halide On a doubly bonded carbon of a chain \(\mathrm{sp^2}\) \(\mathrm{CH_2{=}CH\!-\!X}\)
Haloalkyne On a triply bonded carbon \(\mathrm{sp}\) \(\mathrm{CH{\equiv}C\!-\!X}\)
Aryl halide (haloarene) Directly on an aromatic ring carbon \(\mathrm{sp^2}\) \(\mathrm{C_6H_5\!-\!X}\)

Q. Why should the hybridization of the halogen-bearing carbon deserve a place in the classification at all?

A. Because it controls how tightly the halogen is held. An \(\mathrm{sp^2}\) or \(\mathrm{sp}\) carbon has more s-character, so its bond to halogen is shorter and stronger than the bond from an \(\mathrm{sp^3}\) carbon. In vinylic and aryl halides there is an additional effect — a lone pair on the halogen overlaps with the neighbouring \(\pi\) system — which strengthens the bond still further. This is exactly why alkyl halides react readily with nucleophiles while vinylic and aryl halides resist, as you will see in section 10.6.

Classify each of the following as an alkyl, allylic, benzylic, vinylic, haloalkyne or aryl halide, giving your reason.

(i) \(\mathrm{CH_3\!-\!CH{=}CH\!-\!CH_2\!-\!Cl}\) (ii) \(\mathrm{C_6H_5\!-\!CH(CH_3)\!-\!Br}\) (iii) \(\mathrm{CH_2{=}CH\!-\!Br}\) (iv) \(\mathrm{(CH_3)_3C\!-\!Br}\) (v) 4-chlorotoluene

In every case, first locate the carbon that actually carries the halogen, then decide its hybridization and its surroundings.

  1. The chlorine is on a \(\mathrm{CH_2}\) group that is saturated (\(\mathrm{sp^3}\)) but sits immediately next to the C=C. It is an allylic halide.

  2. The bromine is on an \(\mathrm{sp^3}\) carbon which is directly attached to the benzene ring. It is a benzylic halide; since that carbon also carries one other carbon of the methyl group, it is a secondary benzylic halide.

  3. The bromine is on a carbon of the double bond itself, which is \(\mathrm{sp^2}\). It is a vinylic halide, that is, a haloalkene.

  4. The bromine is on an \(\mathrm{sp^3}\) carbon joined to three methyl groups. It is a tertiary (3°) alkyl halide.

  5. The chlorine is bonded directly to an \(\mathrm{sp^2}\) carbon of the aromatic ring. It is an aryl halide (haloarene).

Classify each of the following, stating the hybridization of the carbon that carries the halogen: (i) \(\mathrm{HC{\equiv}C\!-\!Cl}\), (ii) \(\mathrm{C_6H_5\!-\!CH_2\!-\!CH_2\!-\!Cl}\), (iii) 3-bromocyclohexene, (iv) \(\mathrm{CH_3\!-\!CHI\!-\!CH_3}\).

How This Is Tested

Classification rarely appears as a question by itself. In board and entrance papers it usually turns up as a match-the-following item pairing a structure with its class, or hidden inside a reasoning question — “which of these will not react with aqueous \(\mathrm{KOH}\)?” or “which one undergoes racemization?” — where the first step of the answer is simply to recognise whether the halogen sits on an \(\mathrm{sp^3}\), \(\mathrm{sp^2}\) or \(\mathrm{sp}\) carbon.

Halogen derivatives are not only laboratory and industrial materials — your own body manufactures two of them. The thyroid gland builds the hormones T3 (triiodothyronine) and T4 (thyroxine), both of which are organic molecules carrying iodine atoms bonded to aromatic rings. These hormones set the pace of metabolism in almost every tissue, controlling how fast cells release energy, and they influence growth and brain development in children. The iodine they need has to come from the diet, which is precisely why edible salt in India is fortified with iodine — a deficiency leaves the gland unable to make enough hormone and causes goitre. Before reading further, find the structures of T3 and T4 and count the iodine atoms in each; then predict which of the two you would expect to be the more strongly iodinated.

10.2 Nomenclature of Halogen Derivatives

• In the IUPAC system of nomenclature, does the functional group ‘halogen’ appear as a suffix or a prefix? • What are the trivial names of the laboratory solvents \(\mathrm{CHCl_3}\) and \(\mathrm{CCl_4}\)?

Every halogen derivative can be referred to in two ways — by an older common (trivial) name that chemists have used for generations, and by a systematic IUPAC name that describes the structure precisely. You need both: the common name because bottles, catalogues and older books still carry it, and the IUPAC name because it is the one that can be read backwards to draw the structure.

Common Names

The common names of alkyl halides are built in two words. Name the alkyl group first, then name the halogen as a halide. So \(\mathrm{CH_3\!-\!I}\) is methyl iodide and \(\mathrm{(CH_3)_3C\!-\!Cl}\) is tert-butyl chloride.

IUPAC Names

According to the IUPAC system of nomenclature (Std. XI Chemistry Textbook, Chapter 14, section 14.4.7), alkyl halides are named as haloalkanes. Here the halogen is not treated as a principal functional group at all; it is cited as a substituent prefix — fluoro, chloro, bromo or iodo — placed before the name of the parent alkane. This is why the name never ends in a halogen suffix the way an alcohol ends in -ol.

Aryl halides are named as haloarenes in the common as well as the IUPAC system, so a benzene ring carrying a bromine atom is bromobenzene in both.

For a dihalogen derivative of an arene, the two systems differ in how they state the positions. The common system uses the prefixes o- (ortho), m- (meta) and p- (para), while the IUPAC system uses the numerals 1,2 ; 1,3 and 1,4 respectively. The three arrangements are drawn in Fig. 10.12.

Diagram

Fig. 10.12 – Three benzene rings each bearing two X substituents: adjacent positions labelled ortho (1,2), alternate positions labelled meta (1,3), opposite positions labelled para (1,4); number the ring carbons 1 to 6 on the first ring.

Q. If chlorine is a functional group, why does 2-chloropropane not end in a suffix the way propan-2-ol does?

A. IUPAC ranks functional groups in an order of seniority, and only the senior group of a molecule is expressed as a suffix. Halogens are never given that rank — they are always cited as prefixes. So the parent hydride name stays untouched as propane, and the chlorine is announced in front as 2-chloro.

Building an IUPAC Name

Because the halogen is only a prefix, naming a halogen derivative comes down to naming the parent chain correctly and then attaching the prefix with the right locant. The working sequence is set out in FC 10.2.

Flowchart

FC 10.2 – Writing the IUPAC name of a halogen derivative: identify the longest continuous carbon chain (it must include any C=C or C≡C present) → number the chain from the end that gives the lowest locant to the multiple bond, if there is one; otherwise from the end nearer the first substituent → name the halogen as fluoro/chloro/bromo/iodo with its locant → if the same halogen occurs more than once, use di-, tri-, tetra- → arrange different substituent prefixes in alphabetical order (ignore di-, tri- while alphabetising) → assemble: locant-prefix + parent alkane/alkene/alkyne name.

One point in that sequence is easy to trip over. When the molecule also contains a double or triple bond, the multiple bond is the senior feature and takes the lower number, even if that forces the halogen to a higher number. That is why \(\mathrm{CH_2{=}CH\!-\!CH_2Br}\) is numbered from the double-bond end and is named 3-bromopropene, not 1-bromopropene.

Common and IUPAC names of some halogen derivatives are given in Table 10.1. The last three entries of the table are ring compounds; their structures are drawn in Fig. 10.13.

Table 10.1 Names of some halogen derivatives

Formula Common name IUPAC name
\(\mathrm{CH_2Cl_2}\) Methylene chloride Dichloromethane
\(\mathrm{CH_3CH_2Br}\) Ethyl bromide Bromoethane
\(\mathrm{CH_3CH(Cl)CH_3}\) Isopropyl chloride 2-Chloropropane
\(\mathrm{(CH_3)_2\,CH\!-\!CH_2Br}\) Isobutyl bromide 1-Bromo-2-methylpropane
\(\mathrm{(CH_3)_3\,C\,Br}\) Tert-butyl bromide 2-Bromo-2-methylpropane
\(\mathrm{(CH_3)_3\,C\,CH_2Cl}\) Neopentyl chloride 1-Chloro-2, 2-dimethyl propane
\(\mathrm{CH_2{=}CH\!-\!Cl}\) Vinyl chloride 1-Chloroethene
\(\mathrm{CH_2{=}CH\!-\!CH_2Br}\) Allyl bromide 3-Bromopropene
\(\mathrm{CH{\equiv}C\!-\!Cl}\) Chloro acetylene Chloroethyne
\(\mathrm{C_6H_5CH_2I}\) Benzyl iodide Iodophenylmethane
4-iodo-substituted toluene ring p-Iodotoluene 1-Iodo-4-methyl benzene or 4-Iodotoluene
benzene ring with Cl at 1,3-positions m-dichlorobenzene 1, 3-dichlorobenzene

Diagram

Fig. 10.13 – Three structures matching the last three rows of Table 10.1: benzene ring with –CH₂I (benzyl iodide); benzene ring with CH₃ at position 1 and I at position 4 (p-iodotoluene); benzene ring with Cl at positions 1 and 3 (m-dichlorobenzene).

common name system vs IUPAC name system

Feature Common (trivial) system IUPAC system
How the alkyl halide is built Alkyl group + halide, as two words Halo prefix + parent alkane, as one word
Example Ethyl bromide Bromoethane
Branched chains Named with isopropyl, isobutyl, tert-butyl, neopentyl Named by numbering the longest chain
Position on a benzene ring o-, m-, p- 1,2- ; 1,3- ; 1,4-
Aryl halides Haloarene Haloarene (same)

The trivial name chloroform is a piece of chemical history preserved in a word. The French chemist Jean-Baptiste Dumas, working in the 1830s, found that this liquid gave formic acid on hydrolysis, and coined a name joining chlorine to formyl — the fragment related to formic acid. The everyday name of \(\mathrm{CH_2{=}CH\!-\!Cl}\), vinyl chloride, has an older root still: vinyl comes from the Latin vinum, meaning wine, through the link between this two-carbon fragment and ethyl alcohol.

Write the IUPAC name of each of the following.

(i) \(\mathrm{(CH_3)_2CH\!-\!CH_2\!-\!CH_2\!-\!Br}\) (ii) \(\mathrm{CH_3\!-\!CHCl\!-\!CH_2\!-\!CH_2\!-\!CH_3}\) (iii) \(\mathrm{CH_2{=}CH\!-\!CH_2\!-\!CH_2\!-\!Cl}\) (iv) a benzene ring carrying \(\mathrm{Br}\) and \(\mathrm{Cl}\) at opposite (para) positions

  1. The longest chain running through the carbon that carries bromine has four carbons. Numbering from the \(\mathrm{CH_2Br}\) end puts bromine at C-1 and a methyl branch at C-3. The name is 1-bromo-3-methylbutane.

  2. The chain has five carbons. Numbering from the end nearer the chlorine gives it locant 2 rather than 4, so the name is 2-chloropentane.

  3. Here a double bond is present, and it takes priority in numbering. Numbering from the \(\mathrm{CH_2{=}}\) end makes the alkene begin at C-1 and places chlorine at C-4. The name is 4-chlorobut-1-ene.

  4. On a benzene ring, para positions are 1 and 4. Between bromo and chloro, the alphabetically earlier prefix is given the lower locant, so the name is 1-bromo-4-chlorobenzene.

Write the IUPAC name of each of the following: (i) \(\mathrm{CH_3\!-\!CH_2\!-\!CH(CH_3)\!-\!CH_2\!-\!Br}\), (ii) \(\mathrm{CH_3\!-\!CBr_2\!-\!CH_3}\), (iii) \(\mathrm{CHI_3}\), (iv) a benzene ring carrying two chlorine atoms at adjacent positions.

Write IUPAC names of the following. i. \(\mathrm{CH_3\!-\!CH(Br)\!-\!CH_3}\) ii. \(\mathrm{CH_3\!-\!CH(CH_3)\!-\!CH_2I}\) iii. \(\mathrm{CH_3\!-\!CH{=}CH\!-\!CH_2Cl}\) iv. \(\mathrm{CH_3\!-\!C{\equiv}C\!-\!CH_2\!-\!Br}\) v. a benzene ring carrying one \(\mathrm{Br}\) atom vi. a benzene ring carrying \(\mathrm{Br}\) atoms at the 1 and 4 positions

How This Is Tested

Nomenclature is examined in both directions. A board paper will ask you to write the IUPAC name of a drawn structure, or to draw the structure of a named compound; entrance papers often hide the same skill inside a reaction question, where the product is described by name and you must convert it into a structure before you can go further. Match-the-following items pairing a common name with its IUPAC counterpart — vinyl chloride with 1-chloroethene, allyl bromide with 3-bromopropene — are also common.

Walk along a chemistry store shelf and you will find the same liquid under different labels: a bottle marked methylene chloride is the same substance as one marked dichloromethane, and the industrial degreasing solvent sold as Westrosol is trichloroethylene. Trade names are convenient but they carry no structural information, and two different products can look alike on a label while behaving very differently in a reaction. Before using any halogenated solvent, check the systematic name and the hazard information printed on the bottle rather than relying on the trade name alone — this single habit prevents a large share of laboratory accidents. The same reasoning holds outside the lab: the plastic pipes marked PVC are polyvinyl chloride, made from the vinyl chloride of Table 10.1.

10.3 Methods of Preparation of Alkyl Halides

An alkyl halide can be built in several ways, and the route a chemist chooses depends on what starting material is at hand and how pure the product has to be. The four families of methods covered in this section are collected in FC 10.3.

Flowchart

FC 10.3 – Routes to halogen derivatives: starting material → branch 1: alcohol → (a) halogen acid HX / (b) phosphorus halide PX₃ or PCl₅ / (c) thionyl chloride SOCl₂ → alkyl halide; branch 2: hydrocarbon → alkane + X₂ (light) gives a mixture / alkene + HX gives alkyl halide / alkene + X₂ gives vicinal dihalide → alkyl or dihalogen product; branch 3: another alkyl halide → NaI in acetone (Finkelstein) gives alkyl iodide, metal fluoride (Swartz) gives alkyl fluoride; branch 4: arene → electrophilic halogenation with Lewis acid, or diazonium salt (Sandmeyer) → aryl halide.

10.3.1 From Alcohol

The most widely used method of preparing an alkyl halide is the replacement of the hydroxyl group of an alcohol by a halogen atom. The reason is practical: alcohols are available in a wide variety, so almost any carbon skeleton you need can be bought or made as an alcohol first.

The hydroxyl group may be replaced by a halogen atom using (a) a halogen acid, (b) a phosphorus halide, or (c) thionyl chloride.

By Using a Halogen Acid or Hydrogen Halide (HX)

The conditions for the reaction of an alcohol with a halogen acid (HX) depend on the structure of the alcohol and on the particular halogen acid used. The order of reactivity of alcohols with a given haloacid is \(3^\circ > 2^\circ > 1^\circ\) (refer to section 11.2.1 a).

\[\mathrm{R\!-\!OH} + \mathrm{HX} \xrightarrow{\ \text{suitable condition}\ } \mathrm{R\!-\!X} + \mathrm{H_2O}\]

\[\text{(Alcohol)} \qquad\qquad \text{(Alkyl halide)}\]

Q. Why should a tertiary alcohol react faster than a primary one with the same halogen acid?

A. The acid first protonates the \(\mathrm{-OH}\) group, and the carbon–oxygen bond then has to break so that the halide can take oxygen’s place. As that bond stretches, the carbon begins to carry a positive charge. A tertiary carbon carries three alkyl groups that push electron density towards it and spread that charge out, so the breaking is far easier there than at a primary carbon, which has only one alkyl group to help. Hold on to this idea — the same reasoning returns in section 10.6.4.

Hydrogen chloride is used with zinc chloride (Grooves’ process) for primary and secondary alcohols, but tertiary alcohols readily react with concentrated hydrochloric acid in the absence of zinc chloride.

\[\mathrm{R\!-\!OH} + \mathrm{HCl} \xrightarrow{\ \text{anhydrous }\mathrm{ZnCl_2}\ } \mathrm{R\!-\!Cl} + \mathrm{H_2O}\]

Zinc chloride is a Lewis acid, that is, an electron-pair acceptor, and can therefore coordinate with the oxygen atom of the alcohol. Pulling electron density away from oxygen in this way weakens the \(\mathrm{R\!-\!O}\) bond and makes it easier to break. A mixture of concentrated \(\mathrm{HCl}\) and anhydrous \(\mathrm{ZnCl_2}\) is called Lucas reagent.

Lucas reagent (concentrated \(\mathrm{HCl}\) + anhydrous \(\mathrm{ZnCl_2}\)) (The \(\mathrm{ZnCl_2}\) acts as a Lewis acid and coordinates with the alcohol’s oxygen, weakening the \(\mathrm{R\!-\!O}\) bond → needs no heating for a tertiary alcohol, warming for others → used to convert primary and secondary alcohols into alkyl chlorides, and, because the three classes react at visibly different speeds, also to tell \(1^\circ\), \(2^\circ\) and \(3^\circ\) alcohols apart in the laboratory.)

Constant boiling hydrobromic acid (48%) is used for preparing alkyl bromides. Primary alkyl bromides can also be prepared by reaction with \(\mathrm{NaBr}\) and \(\mathrm{H_2SO_4}\). Here \(\mathrm{HBr}\) is generated in situ, that is, produced inside the reaction mixture itself rather than being added from a bottle.

\[\mathrm{R\!-\!CH_2\!-\!OH} + \mathrm{HBr} \xrightarrow{\ \mathrm{NaBr},\ \mathrm{H_2SO_4},\ \text{heat}\ } \mathrm{R\!-\!CH_2\!-\!Br} + \mathrm{H_2O}\]

A good yield of alkyl iodides may be obtained by heating alcohols with sodium or potassium iodide in 95 % phosphoric acid. Here \(\mathrm{HI}\) is generated in situ.

\[\mathrm{R\!-\!OH} + \mathrm{HI} \xrightarrow{\ \mathrm{NaI}/\mathrm{H_3PO_4}\ } \mathrm{R\!-\!I} + \mathrm{H_2O}\]

Why is phosphoric acid preferred to \(\mathrm{H_2SO_4}\) to prepare \(\mathrm{HI}\) in situ?

By Using a Phosphorus Halide

An alkyl halide may be prepared by the action of a phosphorus halide on an alcohol. Phosphorus tribromide and triiodide are usually generated in situ by the action of red phosphorus on bromine and on iodine respectively. Phosphorus pentachloride reacts with an alcohol to give an alkyl chloride.

\[3\,\mathrm{R\!-\!OH} + \mathrm{PX_3} \rightarrow 3\,\mathrm{R\!-\!X} + \mathrm{H_3PO_3}\]

\[\mathrm{R\!-\!OH} + \mathrm{PCl_5} \rightarrow \mathrm{R\!-\!Cl} + \mathrm{HCl} + \mathrm{POCl_3}\]

Notice the stoichiometry of the first equation: one molecule of \(\mathrm{PX_3}\) can hand over all three of its halogen atoms, so three molecules of alcohol are consumed and phosphorous acid, \(\mathrm{H_3PO_3}\), is left behind.

Sometimes, during the replacement of \(\mathrm{-OH}\) by \(\mathrm{-X}\), alcohols tend to undergo rearrangement — the carbon skeleton quietly reorganises itself and the halogen ends up on the wrong carbon. This tendency can be minimised by the use of phosphorus halides. Straight chain primary alcohols react with a phosphorus trihalide to give unrearranged alkyl halides.

By Using Thionyl Chloride

Thionyl chloride reacts with straight chain primary alcohols to give unrearranged alkyl chloride. The byproducts obtained are gases. There is no need to put extra efforts for its separation, since both simply escape from the reaction vessel. This method is therefore preferred for the preparation of alkyl chlorides.

\[\mathrm{R\!-\!OH} + \mathrm{SOCl_2} \xrightarrow{\ \Delta\ } \mathrm{R\!-\!Cl} + \mathrm{SO_2}\uparrow + \mathrm{HCl}\uparrow\]

thionyl chloride, \(\mathrm{SOCl_2}\) (Replaces \(\mathrm{-OH}\) by \(\mathrm{-Cl}\) on warming → needs dry conditions, since it reacts vigorously with water → used when a clean, unrearranged alkyl chloride is wanted, because the only byproducts, \(\mathrm{SO_2}\) and \(\mathrm{HCl}\), leave as gases and the product needs no further purification.)

HX vs phosphorus halide vs thionyl chloride for converting an alcohol into an alkyl halide

Feature Halogen acid (HX) Phosphorus halide (\(\mathrm{PX_3}\), \(\mathrm{PCl_5}\)) Thionyl chloride (\(\mathrm{SOCl_2}\))
Halide obtained Chloride, bromide or iodide Chloride, bromide or iodide Chloride only
Byproduct Water \(\mathrm{H_3PO_3}\), or \(\mathrm{HCl} + \mathrm{POCl_3}\) \(\mathrm{SO_2}\) and \(\mathrm{HCl}\), both gases
Ease of separation Product must be separated from water and acid Byproducts are liquids or solids and must be removed Byproducts escape on their own
Rearrangement Possible Minimised Avoided with straight chain primary alcohols
Typical use General preparation; \(\mathrm{ZnCl_2}\) needed for \(1^\circ\) and \(2^\circ\) alcohols with \(\mathrm{HCl}\) Preparing bromides and iodides without rearrangement Preferred route to alkyl chlorides

Suggest a suitable reagent for each of the following conversions and write the equation.

(i) Butan-1-ol into 1-chlorobutane, with the chain left unrearranged.

(ii) 2-Methylpropan-2-ol into 2-chloro-2-methylpropane.

(iii) 1-Chlorobutane into 1-iodobutane.

  1. A straight chain primary alcohol is best treated with thionyl chloride, since the product is unrearranged and both byproducts leave as gases.

\[\mathrm{CH_3CH_2CH_2CH_2OH} + \mathrm{SOCl_2} \xrightarrow{\ \Delta\ } \mathrm{CH_3CH_2CH_2CH_2Cl} + \mathrm{SO_2}\uparrow + \mathrm{HCl}\uparrow\]

  1. This is a tertiary alcohol, which reacts readily with concentrated hydrochloric acid without needing zinc chloride.

\[\mathrm{(CH_3)_3C\!-\!OH} + \mathrm{HCl} \rightarrow \mathrm{(CH_3)_3C\!-\!Cl} + \mathrm{H_2O}\]

  1. An alkyl chloride is converted into the iodide by halogen exchange with sodium iodide in acetone.

\[\mathrm{CH_3CH_2CH_2CH_2Cl} + \mathrm{NaI} \xrightarrow{\ \text{acetone}\ } \mathrm{CH_3CH_2CH_2CH_2I} + \mathrm{NaCl}\downarrow\]

Identify the products of the following reactions. i. \(\mathrm{CH_4} + \mathrm{Cl_2} \xrightarrow{\ h\nu\ }\) ? ii. \(\mathrm{CH_3\!-\!CH{=}CH_2} + \mathrm{HCl} \rightarrow\) ? iii. \(\mathrm{CH_3\!-\!CH{=}CH_2} + \mathrm{HBr} \xrightarrow{\ \text{Peroxide}\ }\) ? iv. \(\mathrm{CH_2{=}CH\!-\!CH_3} + \mathrm{Br_2} \xrightarrow{\ \mathrm{CCl_4}\ }\) ?

10.3.2 From Hydrocarbon

Alkyl halides are formed from saturated as well as unsaturated hydrocarbons by various reactions.

Halogenation of Alkanes

Halogenation of alkanes is not suitable for the preparation of alkyl halides, as a mixture of mono and poly halogen compounds is formed. Once one hydrogen has been replaced, the remaining hydrogens of the same molecule are still available for attack, so the reaction does not stop neatly at the monohalogen stage. Separating the resulting mixture is tedious and the yield of any one compound is poor.

Addition of Hydrogen Halide to an Alkene

Alkyl halides are formed on addition of a hydrogen halide to alkenes. Refer to Std. XI Chemistry Textbook, Chapter 15, section 15.2.4 for all the details, including the order of reactivity of HX, Markownikov rule and the peroxide effect.

Three points from that treatment are worth recalling before you attempt the questions below. First, the order of reactivity of the hydrogen halides in this addition is \(\mathrm{HI} > \mathrm{HBr} > \mathrm{HCl}\). Second, when the alkene is unsymmetrical, the two possible products are not formed in equal amounts, and Markownikov’s rule tells you which one dominates. Third, hydrogen bromide alone reverses this preference when peroxides are present.

NotePrinciple / Law

Markownikov’s rule: when an unsymmetrical reagent of the type \(\mathrm{H\!-\!X}\) adds across the double bond of an unsymmetrical alkene, the hydrogen atom attaches itself to that doubly bonded carbon which already carries the greater number of hydrogen atoms, and the halogen goes to the other carbon.

NotePrinciple / Law

Peroxide effect (Kharasch effect): in the presence of peroxide, the addition of \(\mathrm{HBr}\) to an unsymmetrical alkene takes place contrary to Markownikov’s rule, the bromine attaching to the carbon carrying the greater number of hydrogen atoms. The effect is shown by \(\mathrm{HBr}\) only, and not by \(\mathrm{HCl}\) or \(\mathrm{HI}\).

How will you obtain 1-bromo-1-methylcyclohexane from an alkene? Write the possible structures of the alkene and the reaction involved.

The bromine in the product sits on the ring carbon that also carries the methyl group. That carbon must therefore have been one of the two doubly bonded carbons of the starting alkene, and it must be the one that picks up bromine under Markownikov addition. Two alkenes satisfy this requirement, and both are shown in Fig. 10.14.

In the first, 1-methylcyclohexene, the double bond lies inside the ring between the methyl-bearing carbon and its neighbour. Adding \(\mathrm{HBr}\) places hydrogen on the ring carbon carrying one hydrogen and bromine on the carbon carrying the methyl group.

In the second, methylenecyclohexane, the double bond lies between a ring carbon and an exocyclic \(\mathrm{CH_2}\) group. Adding \(\mathrm{HBr}\) places hydrogen on that \(\mathrm{CH_2}\) — converting it into the methyl group of the product — and bromine on the ring carbon.

Both routes therefore converge on the same product, 1-bromo-1-methylcyclohexane.

Diagram

Fig. 10.14 – Two reactions drawn one below the other: (a) 1-methylcyclohexene (cyclohexene ring with CH₃ on one doubly bonded carbon) + HBr → cyclohexane ring bearing CH₃ and Br on the same carbon; (b) methylenecyclohexane (cyclohexane ring with =CH₂ outside the ring) + HBr → the same product; label the product 1-bromo-1-methylcyclohexane in both.

Rewrite the following reactions by filling in the blanks. • \(\mathrm{CH_3\!-\!CH{=}CH_2} + \mathrm{HBr} \rightarrow\) …… + …… (major) (minor) • \(\mathrm{(CH_3)_2C{=}CHCH_3} + \mathrm{HBr} \xrightarrow{\ \text{peroxide}\ }\) …… + …… (major) (minor) • \(\mathrm{CH_3\!-\!CH{=}CH_2} + \mathrm{HBr} \xrightarrow{\ \text{peroxide}\ }\) …… + …… (major) (minor)

Addition of Halogen to an Alkene

Alkenes form an addition product, a vicinal dihalide, with chlorine or bromine, usually in an inert solvent like \(\mathrm{CCl_4}\) at room temperature. The two halogen atoms end up on adjacent carbons, which is exactly what the word vicinal means.

\[\mathrm{R_2C{=}CR_2} + \mathrm{X_2} \xrightarrow{\ \mathrm{CCl_4}\ } \mathrm{R_2CX\!-\!CR_2X} \qquad (\mathrm{X = Cl,\ Br})\]

Allylic Substitution at High Temperature

When alkenes are heated with \(\mathrm{Br_2}\) or \(\mathrm{Cl_2}\) at high temperature, the hydrogen atom of the allylic carbon is substituted with a halogen atom, giving an allyl halide. Note the change of behaviour: at room temperature in \(\mathrm{CCl_4}\) the halogen adds across the double bond, but at high temperature the double bond survives and a hydrogen is replaced instead.

\[\mathrm{CH_2{=}CH\!-\!CH_3} + \mathrm{Cl_2} \rightarrow \mathrm{CH_2{=}CH\!-\!CH_2Cl} + \mathrm{HCl}\]

10.3.3 Halogen Exchange

Alkyl iodides are prepared conveniently by treating alkyl chlorides or bromides with sodium iodide in methanol or acetone solution. The sodium bromide or sodium chloride precipitates from the solution and can be separated by filtration.

\[\mathrm{R\!-\!Cl} + \mathrm{NaI} \xrightarrow{\ \text{acetone}\ } \mathrm{R\!-\!I} + \mathrm{NaCl}\downarrow\]

The reaction is known as the Finkelstein reaction.

Q. Iodide is itself a good leaving group, so why does this exchange not simply reverse itself?

A. Because of the solvent. Sodium iodide dissolves in acetone, but sodium chloride and sodium bromide do not, so as soon as they form they drop out of solution as a precipitate. Removing a product from the reaction mixture keeps pulling the equilibrium forward, and the exchange is driven to completion.

Alkyl fluorides are prepared by heating alkyl chlorides or bromides with metal fluorides such as \(\mathrm{AgF}\), \(\mathrm{Hg_2F_2}\), \(\mathrm{AsF_3}\), \(\mathrm{SbF_3}\) etc.

\[\mathrm{R\!-\!Cl} + \mathrm{AgF} \rightarrow \mathrm{R\!-\!F} + \mathrm{AgCl}\downarrow\]

The reaction is known as the Swartz reaction. Here too an insoluble silver halide precipitates and drives the exchange forward.

Several reactions in this section still carry the names of the chemists who first described them. Hans Finkelstein, a German chemist, reported the iodide exchange in the early 1900s. Frédéric Swarts, a Belgian chemist working in the closing years of the nineteenth century, pioneered the use of metal fluorides such as antimony trifluoride to place fluorine on carbon, opening up the whole field of organofluorine chemistry. Traugott Sandmeyer, a Swiss chemist, discovered his diazonium reaction in the 1880s while working in Victor Meyer’s laboratory — reportedly as a chance observation during another experiment.

Complete each of the following reactions, giving the organic product.

(i) \(3\,\mathrm{CH_3CH_2OH} + \mathrm{PBr_3} \rightarrow\)

(ii) \(\mathrm{CH_3CH_2CH_2OH} + \mathrm{HI} \xrightarrow{\ \mathrm{NaI}/\mathrm{H_3PO_4}\ }\)

(iii) \(\mathrm{CH_3CH_2Br} + \mathrm{AgF} \rightarrow\)

(iv) \(\mathrm{CH_3CH_2CH_2OH} + \mathrm{SOCl_2} \xrightarrow{\ \Delta\ }\)

10.3.4 Electrophilic Substitution

• Identify the product of the following reaction: benzene \(+\ \mathrm{Cl_2} \xrightarrow{\ \text{anhyd. }\mathrm{AlCl_3}\ }\) • Name the type of halide produced in the above reaction. • What type of reactions are shown by benzene?

Aryl chlorides and bromides can be prepared by direct halogenation of benzene and its derivatives through electrophilic substitution. It may be conveniently carried out in the dark at ordinary temperature in the presence of a suitable Lewis acid catalyst like \(\mathrm{Fe}\), \(\mathrm{FeCl_3}\) or anhydrous \(\mathrm{AlCl_3}\). Darkness matters here: light would start a free-radical reaction at the side chain instead of the ring.

When toluene is brominated in the presence of iron, a mixture of ortho and para bromo toluene is obtained, as shown in Fig. 10.15.

\[\mathrm{C_6H_5CH_3} + \mathrm{Br_2} \xrightarrow{\ \mathrm{Fe},\ \text{dark}\ } \mathrm{CH_3C_6H_4Br}\ \text{(ortho and para)} + \mathrm{HBr}\]

Diagram

Fig. 10.15 – Toluene + Br₂ over an arrow marked Fe, dark, giving two products side by side: benzene ring with CH₃ at position 1 and Br at position 2, labelled o-bromotoluene, and benzene ring with CH₃ at position 1 and Br at position 4, labelled p-bromotoluene, plus HBr.

Aromatic electrophilic substitution with iodine is reversible: the hydrogen iodide released can attack the product and undo the reaction. In this case the use of \(\mathrm{HNO_3}/\mathrm{HIO_4}\) removes \(\mathrm{HI}\) by oxidising it to \(\mathrm{I_2}\); with one of the products being continually taken away, the equilibrium is shifted to the right and the iodo product is formed. Fluorine, being highly reactive, is not used this way, so fluoro compounds are not prepared by this method.

10.3.5 Sandmeyer’s Reaction

Aryl halides are most commonly prepared by replacement of the nitrogen of a diazonium salt. A diazonium salt is made from an aromatic amine and carries an \(\mathrm{-N_2^+}\) group, which is an outstandingly good leaving group because it departs as stable nitrogen gas. That is what makes this the standard laboratory route to aryl halides, in contrast with the sluggish direct halogenation described above. (For details refer to Chapter 13, section 13.6.)

How This Is Tested

Preparation methods are examined mainly as conversions and reagent-naming questions: “convert propan-1-ol into 1-iodopropane”, or “name the reagent used to bring about the following conversion”. A second favourite is the multi-step sequence in which compound A becomes B and then C, where each arrow carries only a reagent and you must supply the structures. Keep the reagent and its speciality paired in your mind — \(\mathrm{SOCl_2}\) with clean chlorides, \(\mathrm{NaI}\)/acetone with iodides, metal fluorides with fluorides, diazonium salts with aryl halides — because these are exactly the pairings the questions test.

Several reagents in this section are never stored ready-made, and the reason is safety rather than economy. Phosphorus tribromide and triiodide fume in moist air and are corrosive to skin and glassware, so a chemist prefers to generate them inside the flask by adding red phosphorus to bromine or iodine, using them the instant they are formed. The same logic applies to \(\mathrm{HBr}\) and \(\mathrm{HI}\), both of which are unpleasant gases; generating them in situ from a sodium halide and an acid avoids handling cylinders of them altogether. Thionyl chloride demands its own care: it reacts vigorously with water, releasing \(\mathrm{SO_2}\) and \(\mathrm{HCl}\), so it must be handled with dry apparatus in a fume hood, never at an open bench. Making a reagent where you need it, in the amount you need, is one of the quiet principles of safer and greener laboratory practice.

10.4 Physical Properties

The physical properties of alkyl halides are considerably different from those of the corresponding alkanes. Replacing a single hydrogen atom by a halogen changes how strongly one molecule is pulled towards its neighbours, and that is what physical properties such as boiling point and solubility ultimately measure. The boiling points of alkyl halides are determined by the polarity of the \(\mathrm{C\!-\!X}\) bond as well as by the size of the halogen atom.

10.4.1 Nature of Intermolecular Forces

The halogens (\(\mathrm{X = F,\ Cl,\ Br}\) and \(\mathrm{I}\)) are more electronegative than carbon — that is, they attract the shared pair of a covalent bond more strongly than carbon does.

As a result, the carbon atom that carries the halogen develops a partial positive charge, while the halogen carries a partial negative charge. The carbon–halogen bond in an alkyl halide is therefore a polar covalent bond, and alkyl halides are moderately polar compounds. The separation of charge is drawn in Fig. 10.16.

\[\overset{\delta+}{\mathrm{C}}\!-\!\overset{\delta-}{\mathrm{X}}\]

Diagram

Fig. 10.16 – A carbon atom of a chain bonded to X, with δ⊕ marked above the carbon and δ⊖ above the halogen, and an arrow along the bond pointing from C towards X to show the direction of the dipole.

The size of the halogen atom increases from fluorine to iodine. Hence the \(\mathrm{C\!-\!X}\) bond length increases down the group. The \(\mathrm{C\!-\!X}\) bond strength decreases as the size of the halogen increases. The reason lies in orbital overlap: as the p-orbital of the halogen grows larger it becomes more diffused, its electron density is spread over a bigger region, and the extent of its overlap with the orbital of carbon decreases. A bond built on poorer overlap is a weaker bond.

Some typical bond lengths, bond enthalpies and dipole moments of the \(\mathrm{C\!-\!X}\) bond are given in Table 10.2.

Table 10.2 : Bond parameters of C-X bond

Bond Bond length (pm) Bond enthalpy (kJ mol\(^{-1}\)) Dipole moment (debye)
\(\mathrm{CH_3\!-\!F}\) 139 452 1.847
\(\mathrm{CH_3\!-\!Cl}\) 178 351 1.860
\(\mathrm{CH_3\!-\!Br}\) 193 293 1.830
\(\mathrm{CH_3\!-\!I}\) 214 234 1.636

dipole moment (\(\mu\)) (SI unit: coulomb metre, \(\text{C m}\); the practical unit used in the table is the debye, where \(1\ \text{D} = 3.336\times10^{-30}\ \text{C m}\). It is a vector quantity: by convention the arrow is drawn pointing from the positive end towards the negative end of the bond, that is, from carbon towards halogen. Bond length is quoted in picometres, \(1\ \text{pm} = 10^{-12}\ \text{m}\), and bond enthalpy in \(\text{kJ mol}^{-1}\) — always a positive number, since energy must be supplied to break a bond.)

the C–X bond from fluorine to iodine (Down Group 17 ↓: halogen size increases → \(\mathrm{C\!-\!X}\) bond length increases (139 → 214 pm) because the bonding atoms are bigger; bond enthalpy decreases (452 → 234 kJ mol\(^{-1}\)) because the larger, more diffused p-orbital overlaps less effectively with carbon’s orbital; so \(\mathrm{C\!-\!I}\) is the longest and weakest bond and \(\mathrm{C\!-\!F}\) the shortest and strongest. Remember the consequence rather than the numbers: the weakest bond breaks most easily, which is why iodides are the most reactive alkyl halides and fluorides the least.)

Q. Fluorine is the most electronegative halogen, so why is the dipole moment of \(\mathrm{CH_3F}\) slightly smaller than that of \(\mathrm{CH_3Cl}\)?

A. Because a dipole moment depends on two things — the size of the separated charge and the distance over which it is separated. Fluorine does pull harder, but the \(\mathrm{C\!-\!F}\) bond is much shorter (139 pm against 178 pm), and the shorter distance cancels out the advantage. Beyond chlorine, electronegativity falls away faster than bond length grows, so the dipole moment drops again for \(\mathrm{CH_3Br}\) and \(\mathrm{CH_3I}\).

Q1. A CFC molecule contains both C–Cl and C–F bonds. Why does sunlight break the carbon–chlorine bond and leave the carbon–fluorine bond alone?

A. Compare the two bond enthalpies in Table 10.2. Breaking \(\mathrm{C\!-\!Cl}\) needs \(351\ \text{kJ mol}^{-1}\), while breaking \(\mathrm{C\!-\!F}\) needs \(452\ \text{kJ mol}^{-1}\) — an extra \(101\ \text{kJ mol}^{-1}\). Ultraviolet photons in the upper atmosphere carry enough energy to snap the weaker \(\mathrm{C\!-\!Cl}\) bond but not the stronger \(\mathrm{C\!-\!F}\) one. Fluorine’s small, compact p-orbital overlaps well with carbon and holds on; chlorine’s larger, more diffused orbital does not. So the molecule loses a chlorine atom and keeps its fluorines — and it is that released chlorine atom that goes on to attack ozone.

The unit in the last column of Table 10.2 honours Peter Debye, the Dutch physical chemist whose studies of dipole moments showed that measuring how a substance behaves in an electric field could reveal the shape of its molecules. He received the Nobel Prize in Chemistry in 1936 for this work on molecular structure.

10.4.2 Boiling Point

The boiling points of alkyl halides are considerably higher than those of the corresponding alkanes, due to their higher polarity and higher molecular mass. Two molecules of an alkyl halide attract each other both through their permanent dipoles and through the ordinary van der Waals forces that all molecules feel, so more heat is needed to pull them apart.

Within the alkyl halides, for a given alkyl group, the boiling point increases with increasing atomic mass of the halogen, because the magnitude of the van der Waals force increases with increase in the size and mass of the halogen. A bigger halogen has a larger, looser electron cloud that is more easily distorted, and such a cloud produces stronger momentary attractions between neighbouring molecules.

Thus the boiling point of an alkyl halide decreases in the order

\[\mathrm{RI} > \mathrm{RBr} > \mathrm{RCl} > \mathrm{RF}\]

For example:

Haloalkane \(\mathrm{CH_3F}\) \(\mathrm{CH_3Cl}\) \(\mathrm{CH_3Br}\) \(\mathrm{CH_3I}\)
Boiling point (K) 194.6 248.8 276.6 315.4

For a given halogen, the boiling point rises with increasing carbon number, since a longer chain means a larger surface over which neighbouring molecules can touch and attract one another.

For example,

Haloalkane Boiling point (K)
\(\mathrm{CH_3Cl}\) 248.8
\(\mathrm{CH_3CH_2Cl}\) 285.5
\(\mathrm{CH_3CH_2CH_2Cl}\) 320.0
\(\mathrm{CH_3CH_2CH_2CH_2Cl}\) 351.5

For isomeric alkyl halides, the boiling point decreases with increased branching, as the surface area decreases on branching and the van der Waals forces decrease. A branched molecule is closer to a compact sphere, and spheres touch each other over a smaller area than rods do. For example:

Haloalkane Boiling point (K)
\(\mathrm{CH_3CH_2CH_2CH_2Br}\) 375
\(\mathrm{CH_3\!-\!CHBr\!-\!CH_2\!-\!CH_3}\) 364
\(\mathrm{(CH_3)_3C\!-\!Br}\) 346

Notice that all three compounds in this last table have exactly the same molecular formula and the same molecular mass; only their shape differs. That is what makes them such a clean demonstration of the effect of branching. The relationship between halogen size, bond strength and boiling point is plotted in Fig. 10.17.

Diagram

Fig. 10.17 – A dual plot for CH₃F, CH₃Cl, CH₃Br, CH₃I along the x-axis: left y-axis shows boiling point in K (194.6, 248.8, 276.6, 315.4) as a rising line with points; right y-axis shows C–X bond enthalpy in kJ mol⁻¹ (452, 351, 293, 234) as a falling line with points; label both curves.

the boiling point and bond enthalpy plot of Fig. 10.17 (Study the two curves in Fig. 10.17 and answer: (a) Which quantity rises and which falls as you move from \(\mathrm{CH_3F}\) to \(\mathrm{CH_3I}\)? (b) Both curves are controlled by the same underlying change in the halogen atom — what is it, and why does it push the two properties in opposite directions? (c) Fluoromethane has the strongest \(\mathrm{C\!-\!X}\) bond of the four, yet the lowest boiling point. Explain why there is no contradiction here. (d) Predict roughly where \(\mathrm{CH_3CH_2I}\) would sit on the boiling point curve, and justify your placement.)

Arrange the following compounds in order of increasing boiling points: bromoform, chloromethane, dibromomethane, bromomethane.

The comparative boiling points of halogen derivatives are mainly related with van der Waals forces of attraction, which depend upon the molecular size. In the present case all the compounds contain only one carbon. Thus the molecular size depends upon the size of the halogen and the number of halogen atoms present.

Thus the increasing order of boiling point is,

\[\mathrm{CH_3Cl} < \mathrm{CH_3Br} < \mathrm{CH_2Br_2} < \mathrm{CHBr_3}\]

Read the order once more to see the two rules working one after the other: chlorine is replaced by the larger bromine, and then bromine atoms are added one at a time, each addition enlarging the molecule further.

10.4.3 Solubility

Though alkyl halides are moderately polar, they are insoluble in water. This is due to the inability of alkyl halides to form hydrogen bonds with water. The attraction between alkyl halide molecules is stronger than the attraction between an alkyl halide molecule and a water molecule, so the two liquids stay apart as separate layers rather than mixing. Alkyl halides are soluble in non-polar organic solvents, where the forces they must break and the forces they can form are of comparable strength.

Q2. Alkyl halides are polar molecules, and water is a polar solvent. Why, then, does an alkyl halide refuse to dissolve in water and settle as a separate layer instead?

A. Polarity alone is not enough. For a substance to dissolve in water, the new attractions formed between solute and water must repay the cost of pulling water molecules apart from one another — and water molecules hold each other with hydrogen bonds, which are unusually strong. An alkyl halide has no hydrogen atom attached to a strongly electronegative atom, so it cannot form hydrogen bonds with water at all. Its own molecules attract each other more strongly than water attracts them, so the two liquids separate. In a non-polar organic solvent there are no hydrogen bonds to break in the first place, and the alkyl halide dissolves readily.

Aryl Halides

Aryl halides are also insoluble in water but soluble in organic solvents. If aryl halides are not modified by the presence of any other functional group, they show properties similar to the corresponding alkyl halides.

The isomeric dihalobenzenes have nearly the same boiling points, but the melting points of these isomers show variation. The melting point of the para isomer is quite high compared to that of the ortho or meta isomer. This is because of its symmetrical structure, which can easily pack closely in the crystal lattice. As a result, the intermolecular forces of attraction are stronger and therefore greater energy is required to overcome its lattice energy.

Dichlorobenzene ortho meta para
b.p./K 453 446 448
m.p./K 256 249 323

The contrast in this small table is worth pausing on. Melting is the breaking down of an ordered crystal, so how neatly the molecules stack matters enormously; boiling happens from a liquid in which that order has already been lost, so packing no longer helps. This is exactly why the three isomers differ by nearly \(70\ \text{K}\) in melting point but by only a few kelvin in boiling point.

alkane vs alkyl halide vs aryl halide

Property Alkane Alkyl halide Aryl halide
Polarity of the molecule Non-polar Moderately polar Moderately polar
Boiling point compared with the parent alkane — Considerably higher Comparable to the corresponding alkyl halide
Solubility in water Insoluble Insoluble Insoluble
Solubility in organic solvents Soluble Soluble Soluble
Effect of branching / symmetry Branching lowers boiling point Branching lowers boiling point Symmetry of the para isomer raises the melting point sharply

(i) Which has the higher boiling point, 1-chloropentane or 2-chloro-2-methylbutane? Give a reason. (ii) The boiling points of 1,2-dichlorobenzene and 1,4-dichlorobenzene differ by only a few kelvin, yet their melting points differ by nearly seventy. Explain.

  1. Both compounds have the molecular formula \(\mathrm{C_5H_{11}Cl}\), so they are isomers of equal molecular mass; only the shape differs. 1-Chloropentane is a straight chain, while 2-chloro-2-methylbutane is branched. Branching makes the molecule more compact and reduces its surface area, so neighbouring molecules touch over a smaller region and the van der Waals forces between them are weaker. Less energy is then needed to separate them. Hence 1-chloropentane has the higher boiling point.

  2. Boiling point is decided by the strength of attraction between molecules in the liquid, where the molecules are already disordered; both isomers are similar in size and polarity, so their boiling points are close. Melting point, however, is decided by how well the molecules are locked into a crystal. The para isomer is symmetrical and packs closely and regularly into the lattice, giving strong intermolecular attraction and a high lattice energy, so a much higher temperature is needed to melt it. The ortho isomer is unsymmetrical and packs poorly, and melts far lower.

(i) Arrange \(\mathrm{CH_3F}\), \(\mathrm{CH_3Cl}\), \(\mathrm{CH_3Br}\) and \(\mathrm{CH_3I}\) in increasing order of \(\mathrm{C\!-\!X}\) bond length, and state which of the four has the weakest \(\mathrm{C\!-\!X}\) bond. (ii) Bromoethane does not dissolve in water but dissolves freely in benzene. Give the reason. (iii) Which would you expect to boil at the higher temperature, \(\mathrm{CH_3Cl}\) or \(\mathrm{CH_2Cl_2}\)? Justify your answer.

How This Is Tested

Physical properties are almost always tested as ordering questions — arrange these four halides in increasing order of boiling point — or as short reasoning questions of the “give reasons” type: why are alkyl halides immiscible with water although they are polar; why does the para isomer melt so much higher. In assertion–reason items, the usual trap is to accept a correct statement paired with a wrong explanation, for instance attributing the insolubility of alkyl halides to their being non-polar, which they are not. The safe habit is to name the actual force involved each time — hydrogen bonding, dipole–dipole attraction, van der Waals forces or lattice energy.

The high melting point of the para isomer is not merely a table entry; it is the reason 1,4-dichlorobenzene is sold as a solid in the first place. Its closely packed, symmetrical crystals hold together well enough for it to be moulded into the white blocks used as moth repellents in cupboards and as deodorising blocks in urinals, where it slowly sublimes — passing straight from solid to vapour — and releases its characteristic sharp smell. That same sublimation means you are breathing the compound whenever you smell it, and prolonged exposure in an unventilated room is not advisable; ventilation, and keeping such blocks away from food and from small children, is the sensible precaution. Their gradual disappearance from a cupboard, with no liquid ever left behind, is a small everyday demonstration of sublimation.

10.5 Optical Isomerism in Halogen Derivatives

• What is the relationship between two compounds having the same molecular formula? • What is meant by stereoisomerism?

Isomers having the same bond connectivities, that is, the same structural formula, are called stereoisomers. They are built from the same atoms joined to the same partners; what differs is only the way those atoms are arranged in space.

Knowledge of optical isomerism, which is a kind of stereoisomerism, will be useful to understand the nucleophilic substitution reactions of alkyl halides (see section 10.6.3). There is a good reason to study it here rather than later: the spatial arrangement around a carbon atom turns out to be the most sensitive evidence we have about how a nucleophile attacks that carbon.

10.5.1 Chiral Atom and Molecular Chirality

• Make a three-dimensional model of 2-chlorobutane. • Make another model which is a mirror image of the first model. • Try to superimpose the two models on each other. • Do they superimpose on each other exactly? • Comment on whether the two models are identical or not.

Let us now jot down the atoms and groups attached to each carbon in 2-chlorobutane, numbering the chain from left to right.

\[\overset{1}{\mathrm{C}}\mathrm{H_3}\!-\!\overset{2}{\mathrm{C}}\mathrm{HCl}\!-\!\overset{3}{\mathrm{C}}\mathrm{H_2}\!-\!\overset{4}{\mathrm{C}}\mathrm{H_3}\]

Carbon The four atoms/groups attached to it
C-1 \(\mathrm{-H}\), \(\mathrm{-H}\), \(\mathrm{-H}\), \(\mathrm{-CHCl\!-\!CH_2\!-\!CH_3}\)
C-2 \(\mathrm{-H}\), \(\mathrm{-Cl}\), \(\mathrm{-CH_3}\), \(\mathrm{-CH_2\!-\!CH_3}\)
C-3 \(\mathrm{-H}\), \(\mathrm{-H}\), \(\mathrm{-CH_3}\), \(\mathrm{-CHCl\!-\!CH_3}\)
C-4 \(\mathrm{-H}\), \(\mathrm{-H}\), \(\mathrm{-H}\), \(\mathrm{-CH_2\!-\!CHCl\!-\!CH_3}\)

Run your eye down the table. C-1, C-3 and C-4 each carry at least two identical atoms — two or three hydrogens. It can be seen that the four groups bonded to C-2 are all different from each other.

NoteDefinition

A carbon atom in a molecule which carries four different groups or atoms is called a chiral carbon atom.

Thus, the C-2 in 2-chlorobutane is a chiral carbon. A chiral atom in a molecule is marked with an asterisk (*). For example, \(\mathrm{CH_3\!-\!{}^{*}CHCl\!-\!CH_2\!-\!CH_3}\).

When a molecule contains one chiral atom, it acquires a unique property. Such a molecule cannot superimpose perfectly on its mirror image. It is called a chiral molecule. A chiral molecule and its mirror image are not identical, as shown in Fig. 10.1.

Diagram

Fig. 10.1 : Nonsuperimposable mirror images – A tetrahedral carbon marked with an asterisk bearing CH₃, Cl, C₂H₅ and H, drawn on the left of a vertical mirror plane, with its mirror image drawn on the right; below, the two structures shown overlapped to demonstrate that they do not coincide; label the mirror plane.

A chiral molecule and its mirror image both have the same structural formula and, of course, the same molecular formula. The spatial arrangement of the four different groups around the chiral atom, however, is different. In other words, a chiral molecule and its mirror image are stereoisomers of each other (refer to Std. XI Chemistry Textbook, Chapter 14).

The relationship between a chiral molecule and its mirror image is similar to the relationship between left and right hands. Your two hands have the same parts joined in the same order, and each is the mirror image of the other, yet no amount of turning will make the left hand lie exactly over the right. This is why the property is called handedness or chirality. (Origin : Greek word cheir means hand.)

Figure 10.2 shows a few objects from day to day life which exhibit superimposable and non-superimposable mirror image relationships. A plain glass tumbler and its reflection can be superimposed; a hand or a foot and its reflection cannot.

Diagram

Fig. 10.2 : Superimposable and nonsuperimposable mirror image – Two groups of everyday objects: on the left, a pair of hands and a pair of feet with their mirror images, labelled Non superimposable; on the right, a chair and a drinking glass with their mirror images, labelled Superimposable.

NoteDefinition

The stereoisomerism in which the isomers have different spatial arrangements of groups or atoms around a chiral atom is called optical isomerism.

The optical isomers differ from each other in terms of a measurable property called optical activity. To understand optical activity, we must first know what plane polarized light is.

An important point about the order of discovery is worth remembering here: the phenomenon of optical isomerism in organic compounds was observed first, and its origin in molecular chirality was recognised only later. Chemists could measure the effect for decades before they could explain it.

10.5.2 Plane Polarized Light

Ordinary light consists of electromagnetic waves having oscillations of the electric and magnetic field in all possible planes perpendicular to the direction of propagation of light. Picture the beam coming straight towards you: the vibrations are spread evenly in every direction around the line of travel, like the spokes of a wheel.

When ordinary light is passed through Nicol’s prism, oscillations in only one plane emerge out. The prism behaves like a narrow slit for vibrations, allowing through only those aligned in one direction and blocking the rest.

NoteDefinition

Light having oscillations only in one plane perpendicular to the direction of propagation of light is known as plane polarized light.

The difference between the two kinds of light is drawn in Fig. 10.18.

Diagram

Fig. 10.18 – Cross-section of a beam of ordinary light shown as arrows radiating in all directions within a circle, an arrow passing through a block labelled Nicol Prism, and on the right the cross-section of the emergent beam shown as arrows in a single vertical plane; label the two circles “cross section of ordinary light” and “cross section of plane polarized light”.

A Nicol prism is a special type of prism made from pieces of calcite, a crystalline form of \(\mathrm{CaCO_3}\), arranged in a specific manner. A Nicol prism is also called a polarizer.

10.5.3 Optical Activity

When an aqueous solution of certain organic compounds like sugar or lactic acid is placed in the path of plane polarized light, the transmitted light has oscillations in a different plane than the original. In other words, the incident light undergoes rotation of its plane of polarization. The plane of polarization rotates either to the right (clockwise) or to the left (anticlockwise).

NoteDefinition

The property of a substance by which it rotates the plane of polarization of incident plane polarized light is known as optical activity.

The compounds which rotate the plane of plane polarized light are called optically active compounds, and those which do not rotate it are optically inactive compounds.

Optical activity of a substance is expressed numerically in terms of optical rotation. The angle through which a substance rotates the plane of plane polarized light on passing through it is called optical rotation. The instrument used to measure it is a polarimeter, whose arrangement is shown in Fig. 10.19: light is first polarized, then sent through a tube containing the solution, and a second prism called the analyser is turned until the light passes through it fully once again. The angle through which the analyser had to be turned is the optical rotation.

Diagram

Fig. 10.19 – Schematic of a polarimeter arranged left to right: light source → polarizer (Nicol prism) → plane polarized light → sample tube containing the solution → rotated plane of polarization → analyser (second Nicol prism) marked with a rotation angle α on a circular scale → eyepiece.

In accordance with the direction of optical rotation, an optically active substance is either dextrorotatory or laevorotatory. A compound which rotates the plane of plane polarized light towards the right is called dextrorotatory and is designated by the symbol d- or by a (+) sign. A compound which rotates the plane of plane polarized light towards the left is called laevorotatory and is designated by the symbol l- or by a (−) sign.

Isomerism in which isomeric compounds have different optical activity is known as optical isomerism. The French scientist Louis Pasteur first recognised that optical activity is associated with a certain type of three-dimensional structure of molecules. Pasteur introduced the term enantiomers for the optical isomers having equal and opposite optical rotation.

Three ideas from this subsection should be kept clearly apart in your mind. Optical activity is an experimentally observable property of a compound — you measure it. Chirality is a description of molecular structure — you deduce it from the formula. Optical activity is the consequence of chirality. Molecules which contain one chiral atom are chiral, that is, they are nonsuperimposable on their mirror image; the two non-superimposable mirror image structures are called a pair of enantiomers; and enantiomers have equal and opposite optical rotation, which makes them a kind of optical isomer.

Louis Pasteur was still in his twenties when, around the middle of the nineteenth century, he examined the crystals of a tartrate salt left behind in wine vats. Under the lens he noticed that the crystals came in two kinds, each the mirror image of the other. He separated them by hand with a fine needle, dissolved each pile separately, and found that one solution turned the plane of polarized light to the right and the other turned it by exactly the same angle to the left. It was the first direct demonstration that optical activity has its origin in the shape of molecules. The prism used in such measurements carries the name of William Nicol, the Scottish scientist who devised it from calcite in the 1820s.

Q. If two compounds have exactly the same melting point, boiling point, density and refractive index, how can they possibly be different compounds?

A. Because all of those properties depend on how strongly one molecule attracts another, and mirroring a molecule does not change the strength of those attractions at all. A pair of enantiomers is identical in every such scalar property. The difference shows up only in a measurement that itself has a handedness — the rotation of plane polarized light, which one of them turns to the right and the other by an equal angle to the left — or in a reaction with another chiral, optically active substance, which can tell the two apart just as a right glove can tell your two hands apart.

10.5.4 Enantiomers

NoteDefinition

The optical isomers which are non-superimposable mirror images of each other are called enantiomers, or enantiomorphs, or optical antipodes.

For example, 2-chlorobutane exists as a pair of enantiomers (Fig. 10.1).

Enantiomers have identical physical properties — such as melting point, boiling point, density and refractive index — except the sign of optical rotation. The magnitude of their optical rotation is equal but the sign of optical rotation is opposite. They also have identical chemical properties, except towards an optically active reagent.

An equimolar mixture of enantiomers, that is, of the dextrorotatory and the laevorotatory forms in equal amounts, is called a racemic modification or racemic mixture.

NoteDefinition

A racemic modification is an equimolar mixture of the two enantiomers of a compound, and it is optically inactive.

A racemic modification is optically inactive because the optical rotation due to the molecules of one enantiomer is cancelled by the equal and opposite optical rotation due to the molecules of the other enantiomer. For every molecule turning the plane a little to the right there is another turning it by exactly as much to the left, so the net rotation observed is zero. A racemic modification is designated as (dl) or by the (±) sign.

dextrorotatory vs laevorotatory vs racemic modification

Feature Dextrorotatory form Laevorotatory form Racemic modification
Symbol d- or (+) l- or (−) (dl) or (±)
Direction of rotation To the right (clockwise) To the left (anticlockwise) No net rotation
Magnitude of rotation Equal to that of the l- form Equal to that of the d- form Zero
Optical activity Optically active Optically active Optically inactive
Composition A single enantiomer A single enantiomer Equimolar mixture of both

Q4. Your left hand will not fit into a right-hand glove. What does this everyday fact have to do with the way a molecule of 2-chlorobutane behaves towards a beam of light?

A. Your two hands are mirror images that cannot be laid on top of each other, and the C-2 of 2-chlorobutane creates exactly the same situation in a molecule: it carries four different groups, so the molecule and its mirror image cannot be superimposed. The two forms are enantiomers — a left-handed and a right-handed version of the same compound. This handedness is invisible to melting points and densities, but plane polarized light detects it at once, because light itself can be given a direction of rotation. One enantiomer turns the plane of polarization to the right, the other turns it by an identical angle to the left. Mix them in equal amounts and the two effects cancel, giving an optically inactive racemic mixture — much as a pair of gloves, taken together, shows no overall handedness.

Which of the following molecules are chiral? For each chiral one, mark the chiral carbon with an asterisk and name the four different groups attached to it.

(i) 2-chloropentane (ii) 3-chloropentane (iii) \(\mathrm{C_6H_5\!-\!CHCl\!-\!CH_3}\) (iv) 2-chloro-2-methylpropane

For each compound, find the carbon carrying the chlorine and list the four things attached to it. If all four are different, that carbon is chiral.

  1. In 2-chloropentane, \(\mathrm{CH_3\!-\!CHCl\!-\!CH_2\!-\!CH_2\!-\!CH_3}\), the C-2 carries \(\mathrm{-H}\), \(\mathrm{-Cl}\), \(\mathrm{-CH_3}\) and \(\mathrm{-CH_2CH_2CH_3}\). All four are different, so the molecule is chiral: \(\mathrm{CH_3\!-\!{}^{*}CHCl\!-\!CH_2\!-\!CH_2\!-\!CH_3}\).

  2. In 3-chloropentane, \(\mathrm{CH_3\!-\!CH_2\!-\!CHCl\!-\!CH_2\!-\!CH_3}\), the C-3 carries \(\mathrm{-H}\), \(\mathrm{-Cl}\) and two ethyl groups. Two of the four are identical, so the molecule is not chiral.

  3. The chlorine-bearing carbon holds \(\mathrm{-H}\), \(\mathrm{-Cl}\), \(\mathrm{-CH_3}\) and \(\mathrm{-C_6H_5}\) — four different groups. The molecule is chiral: \(\mathrm{C_6H_5\!-\!{}^{*}CHCl\!-\!CH_3}\).

  4. In 2-chloro-2-methylpropane, \(\mathrm{(CH_3)_3C\!-\!Cl}\), the chlorine-bearing carbon holds three identical methyl groups. The molecule is not chiral.

Note the pattern: a carbon bearing two identical groups can never be chiral, however complicated the rest of the molecule looks.

(i) Mark the chiral carbon with an asterisk in 2-chloro-3-methylbutane and list the four different groups attached to it. (ii) A solution of an optically active compound rotates the plane of polarized light by \(12^\circ\) in the anticlockwise direction. What name and what symbol describe this compound? (iii) What optical rotation would you observe for a solution containing equal numbers of moles of the two enantiomers of 2-chlorobutane, and why?

10.5.5 Representation of Configuration of Molecules

Identify the type of the following 3-D representations (I) and (II) of a molecule and state the significance of the lines drawn. (I) a central carbon written as C with W above, X to the left by a dotted line, Y below, and Z to the right by a solid wedge (II) a cross with W above, Z below, X to the left and Y to the right

Two representations are used to represent the configuration of a chiral carbon and the three-dimensional structure of optical isomers on plane paper. These are (a) the wedge formula and (b) the Fischer projection formula, also called the cross formula (Std. XI Chemistry Textbook, Chapter 14, section 14.2.3). Both exist to solve one problem: a tetrahedral carbon is a three-dimensional object, and the page is flat.

a. Fischer Projection Formula (Cross Formula)

In a Fischer projection the chiral carbon is placed at the point where two lines cross, and it is usually not written at all. The convention that gives the picture its meaning is fixed and must never be broken: the two horizontal lines represent bonds coming above the plane of the paper, towards the viewer, and the two vertical lines represent bonds going below the plane of the paper, away from the viewer. Fig. 10.3 shows both the convention and the tetrahedral structure it stands for.

Diagram

Fig. 10.3 Fischer projection formula – On the left, a cross with Cl at the top, H at the bottom, I on the left arm and Br on the right arm, labelled Fischer projection and with the crossing point marked “chiral carbon”; on the right, the same molecule drawn as a tetrahedral carbon with I and Br on horizontal bonds labelled “Bonds above the plane” and Cl and H on vertical bonds labelled “Bonds below the plane”; caption the pair “Convention of vertical and horizontal lines”.

Q. Why must a Fischer projection never be lifted off the page and turned over?

A. Because the convention fixes which bonds point towards you. Flipping the cross out of the plane of the paper exchanges the horizontal bonds with the vertical ones, so the groups that were coming towards the viewer now go away from the viewer. The picture you get is no longer the same molecule — it is the mirror image, that is, the other enantiomer. A Fischer projection may be rotated within the plane of the paper by \(180^\circ\), but it may never be picked up and flipped.

b. Wedge Formula

When a tetrahedral carbon is imagined to be present in the plane of the paper, all four bonds at this carbon cannot lie in the same plane. Two of them must project out of it, one on each side.

In the wedge formula, the bonds in the plane of the paper are represented by normal lines, the bonds projecting above the plane of the paper are represented by solid wedges (or simply by bold lines), while the bonds going below the plane of the paper are represented by broken wedges (or simply by broken lines). The three kinds of line are shown in Fig. 10.20.

Diagram

Fig. 10.20 – A central carbon with four bonds: Br drawn upward as a normal line labelled “In the plane”, I drawn to the left as a broken wedge labelled “below the plane”, Cl drawn to the right as a normal line, and H drawn downward as a solid wedge labelled “Above the plane”.

wedge formula vs Fischer projection formula

Feature Wedge formula Fischer projection formula
How the chiral carbon appears Drawn explicitly at the centre Understood at the crossing point, usually not written
Bonds towards the viewer Solid wedge or bold line Both horizontal lines
Bonds away from the viewer Broken wedge or broken line Both vertical lines
Bonds in the plane of paper Normal lines Not shown separately
Chief advantage Looks like the real tetrahedral shape Quick to draw and compare, especially for long chains
  1. Draw structures of the enantiomers of lactic acid, \(\mathrm{CH_3\!-\!CH(OH)\!-\!COOH}\), using Fischer projection formulae.
  2. Draw structures of the enantiomers of 2-bromobutane using wedge formulae.
How This Is Tested

The commonest question types are: identify the chiral molecule from a list of four; mark the chiral carbon in a given structure; draw the enantiomers of a named compound using Fischer or wedge formulae; and explain optical isomerism in a specific compound such as 2-chlorobutane. Assertion–reason items often pair a true statement about enantiomers having identical physical properties with a wrong reason, so check both halves separately. In the next section, chirality becomes a diagnostic tool rather than a topic in itself — whether a product turns out optically active or racemic will tell you which mechanism the reaction followed.

Optical rotation is measured every day in the sugar industry. Because sucrose solutions rotate plane polarized light by an amount proportional to their concentration, a polarimeter reading gives the sugar content of cane juice or of a syrup within minutes and without destroying the sample, which is why the instrument is a fixture in sugar mills and quality-control laboratories. Chirality also matters enormously in medicine, since the receptors in our bodies are themselves chiral and can distinguish between the two enantiomers of a drug just as a hand distinguishes gloves. The most sobering example is thalidomide, marketed in the late 1950s to relieve morning sickness: one enantiomer produced the intended calming effect while the other was found to cause severe birth defects, and thousands of children were affected before the drug was withdrawn in the early 1960s. That tragedy is the reason modern regulations require the two enantiomers of a chiral drug to be tested separately, and it is why so much effort now goes into synthesising a medicine as a single, pure enantiomer rather than as a racemic mixture.

10.6 Chemical Properties

10.6.1 Laboratory Test of Haloalkanes

Haloalkanes are of neutral type in aqueous medium — they neither turn litmus red nor blue, so acidity or basicity gives no clue to their presence. Their halogen is locked into a covalent bond and therefore does not exist as a free ion in solution, which is why a fresh sample of an alkyl halide gives no precipitate with silver nitrate directly.

The test therefore begins by breaking that covalent bond. On warming with aqueous sodium or potassium hydroxide, the covalently bonded halogen in the haloalkane is converted to halide ion.

\[\mathrm{R\!-\!X} + \mathrm{OH^-} \xrightarrow{\ \Delta\ } \mathrm{R\!-\!OH} + \mathrm{X^-}\]

When this reaction mixture is acidified by adding dilute nitric acid, and silver nitrate solution is added, a precipitate of silver halide is formed, which confirms the presence of halogen in the original organic compound.

\[\mathrm{Ag^+}\text{(aq)} + \mathrm{X^-}\text{(aq)} \rightarrow \mathrm{AgX}\downarrow\text{(s)}\]

The dilute nitric acid is added first for a practical reason: it neutralises the excess alkali, which would otherwise precipitate silver oxide and spoil the test.

10.6.2 Nucleophilic Substitution Reactions of Haloalkanes

• What is meant by a substitution reaction? • Can you identify the substitution reaction from the following? (i) \(\mathrm{CH_3\!-\!CH_2\!-\!OH} + \mathrm{HCl} \xrightarrow{\ \mathrm{ZnCl_2}\ } \mathrm{CH_3\!-\!CH_2\!-\!Cl} + \mathrm{H_2O}\) (ii) \(\mathrm{CH_2{=}CH_2} + \mathrm{HI} \rightarrow \mathrm{CH_3\!-\!CH_2\!-\!I}\) • Is the carbon carrying the halogen in an alkyl halide an electrophilic or a nucleophilic centre?

NoteDefinition

When a group bonded to a carbon in a substrate is replaced by another group to give a product with no change in the state of hybridization of that carbon, the reaction is called a substitution reaction.

The \(\mathrm{C\!-\!X}\) bond in alkyl halides is a polar covalent bond, and the carbon in the \(\mathrm{C\!-\!X}\) bond is positively polarized. In other words, the \(\mathrm{C\!-\!X}\) carbon is an electrophilic centre — a site short of electron density, hungry for a pair of electrons. It has, therefore, a tendency to react with a nucleophile (refer to Std. XI Chemistry Textbook, Chapter 14).

NoteDefinition

A nucleophile is a species that uses its own electron pair to form a bond with carbon; an electrophile is a species that accepts an electron pair.

Alkyl halides react with a variety of nucleophiles to give nucleophilic substitution reactions, written in short as \(\mathrm{S_N}\). The reaction is represented in general form as shown below.

\[\mathrm{Nu^-} + \overset{\delta+}{\mathrm{C}}\!-\!\overset{\delta-}{\mathrm{X}} \longrightarrow \mathrm{C\!-\!Nu} + \mathrm{X^-}\]

When a substrate reacts fast it is said to be reactive. The reactivity of alkyl halides in an \(\mathrm{S_N}\) reaction depends upon two factors, namely, the substitution state (\(1^\circ\), \(2^\circ\) or \(3^\circ\)) of the carbon and the nature of the halogen. The order of reactivity influenced by these two factors is as shown below.

\[\text{tertiary }(3^\circ) > \text{secondary }(2^\circ) > \text{primary }(1^\circ)\]

\[\mathrm{R\!-\!I} > \mathrm{R\!-\!Br} > \mathrm{R\!-\!Cl}\]

The second of these orders should feel familiar from section 10.4.1: the \(\mathrm{C\!-\!I}\) bond is the longest and weakest of the three, so it breaks most readily and the iodide leaves most easily.

reactivity of alkyl halides towards nucleophilic substitution (With the halogen changed, \(\mathrm{R\!-\!I} > \mathrm{R\!-\!Br} > \mathrm{R\!-\!Cl}\) because the \(\mathrm{C\!-\!X}\) bond enthalpy falls from 351 to 234 kJ mol\(^{-1}\), so the weakest bond breaks fastest. With the carbon skeleton changed, overall reactivity runs \(3^\circ > 2^\circ > 1^\circ\) — but for a specific reason that depends on the mechanism, as section 10.6.4 will show: tertiary halides win by the \(\mathrm{S_N}1\) route, while primary halides are the fastest by the \(\mathrm{S_N}2\) route.)

Examples of some important nucleophilic substitution reactions of alkyl halides are shown in Table 10.3. Read the table as a toolkit: each row tells you which reagent converts an alkyl halide into which class of compound, and together they explain why alkyl halides are such valuable starting materials.

Table 10.3 Nucleophilic substitution reactions of alkyl halides

Sr. No. Alkyl halide Reagent Substitution product
1. \(\mathrm{R\!-\!X}\) \(\mathrm{NaOH}\)(aq) (or \(\mathrm{KOH}\)), \(\Delta\) \(\mathrm{R\!-\!OH}\) (alcohol) \(+\ \mathrm{NaX}\) (or \(\mathrm{KX}\))
2. \(\mathrm{R\!-\!X}\) \(\mathrm{NaOR'}\) (sodium alkoxide), \(\Delta\) \(\mathrm{R\!-\!O\!-\!R'}\) (ether) \(+\ \mathrm{NaX}\)
3. \(\mathrm{R\!-\!X}\) \(\mathrm{R'COOAg}\) (silver carboxylate), \(\Delta\) \(\mathrm{R'COOR}\) (ester) \(+\ \mathrm{AgX}\downarrow\)
4. \(\mathrm{R\!-\!X}\) \(\mathrm{NH_3}\)(alc.) in excess, \(\Delta\), pressure \(\mathrm{R\!-\!NH_2}\) (primary amine) \(+\ \mathrm{HX}\)
5. \(\mathrm{R\!-\!X}\) \(\mathrm{KCN}\) (alc.), \(\Delta\) \(\mathrm{R\!-\!CN}\) (nitrile / alkyl cyanide) \(+\ \mathrm{KX}\)
6. \(\mathrm{R\!-\!X}\) \(\mathrm{AgCN}\) (alc.), \(\Delta\) \(\mathrm{R\!-\!N{\equiv}C}\) (isocyanide) \(+\ \mathrm{AgX}\downarrow\)
7. \(\mathrm{R\!-\!X}\) \(\mathrm{KO\!-\!N{=}O}\) (potassium nitrite) \(\mathrm{R\!-\!O\!-\!N{=}O}\) (alkyl nitrite) \(+\ \mathrm{KX}\)
8. \(\mathrm{R\!-\!X}\) \(\mathrm{Ag\!-\!O\!-\!N{=}O}\) (silver nitrite) \(\mathrm{R\!-\!NO_2}\) (nitroalkane) \(+\ \mathrm{AgX}\downarrow\)
Ambident Nucleophiles

Look carefully at rows 5 and 6, and again at rows 7 and 8. In each pair the same element of the nucleophile is present, yet the products are quite different compounds. The explanation lies in a special class of nucleophile.

The cyanide ion is capable of attacking through more than one site (atom), because its negative charge is shared between carbon and nitrogen, as the resonance structures in Fig. 10.21 show.

Diagram

Fig. 10.21 – Resonance structures of the two ambident nucleophiles: (a) ⁻:C≡N: ↔︎ :C=N:⁻ with the lone pairs and negative charge marked on carbon and on nitrogen; (b) nitrite ion ⁻O–N=O ↔︎ O=N–O⁻ showing the negative charge shared between the two oxygen atoms and the lone pair on nitrogen.

Such nucleophiles are called ambident nucleophiles. \(\mathrm{KCN}\) is predominantly ionic (\(\mathrm{K^+ \ C{\equiv}N^-}\)) and provides cyanide ions. Both carbon and nitrogen are capable of donating an electron pair. The \(\mathrm{C\!-\!C}\) bond being stronger than the \(\mathrm{C\!-\!N}\) bond, attack occurs through the carbon atom of the cyanide group, forming alkyl cyanides as the major product.

However, \(\mathrm{AgCN}\) (\(\mathrm{Ag\!-\!C{\equiv}N}\)) is mainly a covalent compound. Its carbon is already tied up in the bond to silver, and the nitrogen is free to donate a pair of electrons. Hence attack occurs through nitrogen, resulting in the formation of isocyanide.

Another ambident nucleophile is the nitrite ion, which can attack through ‘O’ or ‘N’.

\(\mathrm{KCN}\) versus \(\mathrm{AgCN}\) (Both supply the cyanide group → \(\mathrm{KCN}\) is ionic and free cyanide attacks through its carbon; \(\mathrm{AgCN}\) is largely covalent and attacks through its nitrogen → use alcoholic \(\mathrm{KCN}\) when you want an alkyl cyanide, \(\mathrm{R\!-\!CN}\), which can later be hydrolysed to a carboxylic acid or reduced to an amine; use alcoholic \(\mathrm{AgCN}\) when you want the isocyanide, \(\mathrm{R\!-\!NC}\). The same ionic-versus-covalent reasoning applies to \(\mathrm{KNO_2}\) and \(\mathrm{AgNO_2}\).)

Alkyl halides when treated with an alcoholic solution of silver nitrite give nitroalkanes, whereas with sodium nitrite they give alkyl nitrites. Explain.

10.6.3 Mechanism of \(\mathrm{S_N}\) Reaction

• What is meant by order and molecularity of a reaction? • What is meant by the mechanism of a chemical reaction?

It can be seen from Table 10.3 that in nucleophilic substitution reactions of alkyl halides the halogen atom gets detached from the carbon, and a new bond is formed between that electrophilic carbon and the nucleophile. The covalently bonded halogen is converted into a halide ion (\(\mathrm{X^-}\)). It means that the two electrons constituting the original covalent bond are carried away by the halogen along with it. The halogen atom of the alkyl halide is therefore called the leaving group in the context of this reaction.

NoteDefinition

A leaving group is the group which leaves the carbon by taking away the bond pair of electrons with it.

The substrate undergoes two changes during an \(\mathrm{S_N}\) reaction. The original \(\mathrm{C\!-\!X}\) bond undergoes heterolysis — an unequal splitting in which one atom takes both electrons — and a new bond is formed between the carbon and the nucleophile using two electrons of the nucleophile. These changes may occur in one or more steps.

NoteDefinition

The description regarding the sequence and the way in which these two changes take place in an \(\mathrm{S_N}\) reaction is called the mechanism of the \(\mathrm{S_N}\) reaction.

The mechanism is deduced from the results of the study of the kinetics of \(\mathrm{S_N}\) reactions. This is an important point of method: nobody has ever watched a single molecule react, so the evidence is indirect. What chemists measure is how the rate responds when the concentration of each reactant is changed, and from that they reason backwards to the sequence of events. Two mechanisms are observed in various \(\mathrm{S_N}\) reactions. These are denoted as \(\mathrm{S_N}1\) and \(\mathrm{S_N}2\) mechanisms.

a. \(\mathrm{S_N}2\) Mechanism

The reaction between methyl bromide and hydroxide ion to give methanol follows second order kinetics, that is, the rate of this reaction depends on the concentration of two reacting species, namely, methyl bromide and hydroxide. Hence it is called substitution nucleophilic bimolecular, \(\mathrm{S_N}2\).

\[\mathrm{CH_3Br} + \mathrm{OH^-} \longrightarrow \mathrm{CH_3OH} + \mathrm{Br^-}\]

\[\text{rate} = k\,[\mathrm{CH_3Br}]\,[\mathrm{OH^-}]\]

The rate of a chemical reaction is influenced by the chemical species taking part in the slowest step of its mechanism. In the above reaction only two reactants are present and both are found to influence the rate of the reaction. This means that the reaction is a single step reaction, which can also be called the slow step. This further implies that the two changes, namely, bond breaking and bond forming at the carbon, take place simultaneously. This \(\mathrm{S_N}2\) mechanism is represented as shown in Fig. 10.4.

Diagram

Fig. 10.4 : S_N2 mechanism – HO⁻ approaching the carbon of CH₃Br from the side opposite to Br, with a curly arrow from the lone pair of OH⁻ to carbon and another curly arrow from the C–Br bond to Br; the transition state drawn in square brackets with HO···C···Br collinear, each of HO and Br carrying ½⊖, and the three C–H bonds in one plane at 120°; the product HO–CH₃ drawn with the three hydrogens swung over to the opposite side, plus Br⁻; label the transition state (T.S.) and mark the umbrella-like inversion.

Salient features of the \(\mathrm{S_N}2\) mechanism:

  1. Single step mechanism with simultaneous bond breaking and bond forming.

  2. Backside attack of the nucleophile: The nucleophile attacks the carbon undergoing substitution from the side opposite to that of the leaving group. This is to avoid steric repulsion (repulsion due to bulkiness of the groups) and electrostatic repulsion between the incoming nucleophile and the leaving group.

  3. In the transition state (T.S.) the nucleophile and the leaving group are bonded to the carbon with partial bonds and carry partial negative charge, so the total negative charge is diffused, that is, spread out rather than concentrated at one point. A spread-out charge means a lower-energy arrangement, which is why such a crowded structure can exist at all.

  4. The T.S. contains pentacoordinate carbon having three \(\sigma\) (sigma) bonds in one plane making bond angles of \(120^\circ\) with each other, and two partial covalent bonds along a line perpendicular to this plane. Note that this carbon is not forming five full bonds; two of the five are half-made and half-broken, which is exactly what makes the transition state a fleeting arrangement rather than a compound you could bottle.

  5. When an \(\mathrm{S_N}2\) reaction is brought about at a chiral carbon (in an optically active substrate), the product is found to have the opposite configuration compared to that of the substrate. In other words, the \(\mathrm{S_N}2\) reaction is found to proceed with inversion of configuration. This is like the flipping of an umbrella in a strong wind (see Fig. 10.4). It is known as Walden inversion. The inversion in configuration is the result of the backside attack of the nucleophile.

NoteDefinition

Walden inversion is the turning inside out of the configuration at a chiral carbon during an \(\mathrm{S_N}2\) reaction, so that the product has the configuration opposite to that of the substrate.

Flowchart

FC 10.4 – S_N2 mechanism: R–X + Nu⁻ → nucleophile approaches from the side opposite the leaving group → single transition state with pentacoordinate carbon, partial Nu···C and C···X bonds, ½⊖ on each → simultaneous bond formation and bond breaking → R–Nu + X⁻; branch: if the carbon is chiral → product has inverted configuration (Walden inversion).

Q. The word ‘bimolecular’ counts two species. Why does that force the reaction to be a single-step one?

A. Because molecularity counts the species that come together in the slow step, and the rate law tells you exactly which those are. Here both the alkyl halide and the hydroxide ion appear in the rate law, so both must be present in the slow step. If the mechanism had two steps, only the reactants of the slower one would show up in the rate law. With only two reactants and both of them in the rate law, there is nothing left for a second step to do — so the single step is itself the slow step.

Diagram

Fig. 10.22 – Two graphs side by side, each with concentration of nucleophile [Nu⁻] on the x-axis and reaction rate on the y-axis: graph (a) labelled reaction of CH₃Br with OH⁻ shows a straight line rising through the origin; graph (b) labelled reaction of (CH₃)₃CBr with OH⁻ shows a horizontal line independent of [Nu⁻].

the two rate plots of Fig. 10.22 (Look at Fig. 10.22 and answer: (a) In which of the two reactions does doubling the hydroxide concentration double the rate? (b) What is the order of each reaction with respect to the nucleophile, and what does the horizontal line in graph (b) tell you about whether the nucleophile takes part in the slow step? (c) Deduce which graph belongs to a single-step mechanism and which to a two-step mechanism, and give your reasoning. (d) If the substrate in graph (b) were replaced by a primary halide, sketch how the plot would change.)

b. \(\mathrm{S_N}1\) Mechanism

The reaction between tert-butyl bromide and hydroxide ion to give tert-butyl alcohol follows first-order kinetics, that is, the rate of this reaction depends on the concentration of only one species, which is the substrate molecule, tert-butyl bromide. Hence it is called substitution nucleophilic unimolecular, \(\mathrm{S_N}1\).

\[\mathrm{(CH_3)_3C\!-\!Br} + \mathrm{OH^-} \longrightarrow \mathrm{(CH_3)_3C\!-\!OH} + \mathrm{Br^-}\]

\[\text{rate} = k\,[\mathrm{(CH_3)_3CBr}]\]

It can be seen in this reaction that the concentration of only the substrate appears in the rate equation; the concentration of the nucleophile does not influence the reaction rate. In other words, tert-butyl bromide reacts with hydroxide by a two step mechanism. In the slow step the \(\mathrm{C\!-\!X}\) bond in the substrate undergoes heterolysis, and in the subsequent fast step the nucleophile uses its electron pair to form a new bond with the carbon undergoing change. This \(\mathrm{S_N}1\) mechanism is represented as shown in Fig. 10.5.

Step I

\[\mathrm{(CH_3)_3C\!-\!Br} \xrightarrow{\ \text{slow}\ } \mathrm{(CH_3)_3C^+} + \mathrm{Br^-}\]

Step II

\[\mathrm{(CH_3)_3C^+} + \mathrm{OH^-} \xrightarrow{\ \text{fast}\ } \mathrm{(CH_3)_3C\!-\!OH}\]

Diagram

Fig. 10.5 : S_N1 mechanism – Step I: (CH₃)₃C–Br with a curly arrow from the C–Br bond to Br, over a slow, reversible double arrow, giving the planar carbocation (CH₃)₃C⁺ drawn with three methyl groups at 120° in one plane, plus Br⁻; label “carbocation intermediate”. Step II: the planar carbocation with OH⁻ approaching, giving (CH₃)₃C–OH; show that OH⁻ can approach from either face of the plane.

Salient features of the \(\mathrm{S_N}1\) mechanism:

  1. Two step mechanism.

  2. Heterolysis of the \(\mathrm{C\!-\!X}\) bond in the slow and reversible first step to form a planar carbocation intermediate.

  3. Attack of the nucleophile on the carbocation intermediate in the fast second step to form the product.

  4. When an \(\mathrm{S_N}1\) reaction is carried out at a chiral carbon in an optically active substrate, the product formed is nearly racemic. This indicates that the \(\mathrm{S_N}1\) reaction proceeds mainly with racemization. This means both the enantiomers of the product are formed in almost equal amount. Racemization in an \(\mathrm{S_N}1\) reaction is the result of the formation of the planar carbocation intermediate (Fig. 10.5). The nucleophile can attack the planar carbocation from either side, which results in the formation of both the enantiomers of the product.

Flowchart

FC 10.5 – S_N1 mechanism: R–X → slow, reversible heterolysis of the C–X bond → planar carbocation R⁺ + X⁻ → fast attack by Nu⁻ → R–Nu; branch at the carbocation: attack from the top face gives one enantiomer, attack from the bottom face gives the other → nearly racemic product when the carbon is chiral.

Q. If the carbocation is truly planar, why is the product described as nearly racemic rather than exactly racemic?

A. Because the halide ion that has just left does not move away instantly. For a very short time it stays close to the face of the carbocation it departed from, partly shielding that side. The nucleophile therefore finds the opposite face slightly more accessible, and a small excess of the inverted product is usually obtained. The two faces are equal in principle, but not quite equal in practice — hence “nearly”.

Q5. Two alkyl halides are treated with hydroxide ion. For one of them, the rate depends on how concentrated the hydroxide is; for the other, it does not matter at all. How can the same kind of reaction behave in two such different ways?

A. Because the two halides reach the same destination by different routes. With methyl bromide, the hydroxide ion and the substrate must meet in a single step, so both concentrations appear in the rate law and doubling the hydroxide doubles the rate — the \(\mathrm{S_N}2\) route. With tert-butyl bromide, the slow step is the substrate breaking apart on its own into a carbocation and a bromide ion; the hydroxide is not present at that moment and only pounces afterwards, in a fast step. Since the rate is set entirely by the slow step, adding more hydroxide changes nothing — the \(\mathrm{S_N}1\) route. The overall reaction and the product look the same; the sequence of events does not. And the two routes leave different fingerprints on a chiral substrate: inversion for \(\mathrm{S_N}2\), near-racemization for \(\mathrm{S_N}1\).

The inversion described in feature (v) carries the name of Paul Walden, a chemist born in what is now Latvia, who reported in the closing years of the nineteenth century that a series of substitutions could convert an optically active acid into its mirror-image form and back again. He could not explain how a molecule turned inside out, and the puzzle stood for decades until the backside attack of the nucleophile was worked out — a good example of an observation waiting a long time for its mechanism.

• Draw the Fischer projection formulae of the two products obtained when compound (A) reacts with \(\mathrm{OH^-}\) by the \(\mathrm{S_N}1\) mechanism, where (A) is \(\mathrm{H_3C\!-\!C(C_2H_5)(n\text{-}C_3H_7)\!-\!Br}\). • Draw the Fischer projection formula of the product formed when compound (B) reacts with \(\mathrm{OH^-}\) by the \(\mathrm{S_N}2\) mechanism, where (B) is \(\mathrm{H\!-\!C(CH_3)(C_2H_5)\!-\!Cl}\).

\(\mathrm{S_N}1\) vs \(\mathrm{S_N}2\) mechanism

Feature \(\mathrm{S_N}1\) \(\mathrm{S_N}2\)
Number of steps Two One
Kinetics First order Second order
Rate law rate \(= k\,[\mathrm{RX}]\) rate \(= k\,[\mathrm{RX}][\mathrm{Nu^-}]\)
Molecularity of the slow step Unimolecular Bimolecular
Intermediate or transition state Planar carbocation intermediate Pentacoordinate transition state, no intermediate
Bond breaking and bond forming Occur separately, breaking first Occur simultaneously
Effect of nucleophile concentration None Rate rises with it
Stereochemical outcome at a chiral carbon Mainly racemization Inversion of configuration (Walden inversion)
Substrate most favoured Tertiary halide Primary halide
Example \(\mathrm{(CH_3)_3C\!-\!Br} + \mathrm{OH^-}\) \(\mathrm{CH_3Br} + \mathrm{OH^-}\)

10.6.4 Factors Influencing \(\mathrm{S_N}1\) and \(\mathrm{S_N}2\) Mechanism

a. Nature of Substrate

\(\mathrm{S_N}2\) : The transition state of the \(\mathrm{S_N}2\) mechanism is pentacoordinate and thus crowded (see Fig. 10.4). Every extra alkyl group on the reacting carbon adds bulk to an already congested arrangement, raising its energy and slowing the reaction. As a result, the \(\mathrm{S_N}2\) mechanism is favoured in primary halides and least favoured in tertiary halides.

\(\mathrm{S_N}1\) : A planar carbocation intermediate is formed in the \(\mathrm{S_N}1\) reaction. It has no steric crowding, since only three groups surround the carbon and they lie flat at \(120^\circ\) to one another. Bulky alkyl groups can be easily accommodated in a planar carbocation (see Fig. 10.5). As a result, the \(\mathrm{S_N}1\) mechanism is most favoured in tertiary halides and least favoured in primary halides. Formation of the planar carbocation intermediate in fact results in a relief from the steric crowding present in the tertiary halide substrate.

Secondly, the carbocation intermediate is stabilized by the \(+\mathrm{I}\) effect of alkyl substituents — their tendency to push electron density towards the electron-deficient carbon — and also by the hyperconjugation effect of alkyl substituents containing \(\alpha\)-hydrogens. The more alkyl groups there are, the more help of both kinds the positive carbon receives. As a result, the \(\mathrm{S_N}1\) mechanism is most favoured in tertiary halides and least favoured in primary halides. Both effects are drawn out in Fig. 10.6, and the resulting opposite trends are summarised in Fig. 10.23.

Diagram

Fig. 10.6 : Influence of substrate in S_N1 and S_N2 – Row (a) Transition states in S_N2: four pentacoordinate transition states drawn in a row for CH₃X, primary, secondary and tertiary substrates, with Nu···C···X collinear and ½⊖ on each end, the number of alkyl groups increasing left to right, under a long arrow labelled “crowding and destabilization increases”. Row (b) Carbocation intermediates in S_N1: four planar carbocations for the same four substrates, α-hydrogens marked, under a long arrow labelled “steric relief, stabilization by +I and hyperconjugation of α-hydrogens increases”.

Diagram

Fig. 10.23 – A horizontal line of substrates CH₃–X, 1°, 2°, 3° with an arrow above pointing right labelled “S_N1 rate increases” and an arrow below pointing left labelled “S_N2 rate increases”.

Tertiary halides undergo nucleophilic substitution by the \(\mathrm{S_N}1\) mechanism, while primary halides follow the \(\mathrm{S_N}2\) mechanism. Secondary halides react by either of the mechanisms, or by a mixed mechanism, depending upon the exact conditions.

Primary allylic and primary benzylic halides show higher reactivity by the \(\mathrm{S_N}1\) mechanism than other primary alkyl halides. Explain.

The \(\mathrm{S_N}1\) reaction involves the formation of a carbocation intermediate. The allylic and benzylic carbocation intermediates formed are resonance stabilized, and hence the \(\mathrm{S_N}1\) mechanism is favoured. In the allylic carbocation the positive charge is shared between two carbon atoms; in the benzylic carbocation it is spread into the ring as well. A charge that is shared over several atoms is a charge that costs less energy to create, so these carbocations form far more readily than an ordinary primary carbocation could. The resonance structures are drawn in Fig. 10.24.

\[\mathrm{CH_2{=}CH\!-\!\overset{+}{C}H_2} \longleftrightarrow \mathrm{\overset{+}{C}H_2\!-\!CH{=}CH_2}\]

Diagram

Fig. 10.24 – Two panels: (a) Resonance stabilization of the allylic carbocation, showing CH₂=CH–CH₂⁺ ↔︎ ⁺CH₂–CH=CH₂ with curly arrows for the shift of the π electrons; (b) Resonance stabilization of the benzylic carbocation, showing C₆H₅–CH₂⁺ and its four resonance structures in which the positive charge appears at the ortho and para ring carbons, with curly arrows drawn on each.

b. Nucleophilicity of the Reagent

• Give some examples of nucleophiles that are electrically neutral. • Give some examples of anionic nucleophiles. • What is the difference between a base and a nucleophile?

A nucleophile is a species that uses its electron pair to form a bond with carbon. The nucleophilic character of any species is expressed in its electron releasing tendency, which can be correlated to its strength as a Lewis base.

A more powerful nucleophile attacks the substrate faster and favours the \(\mathrm{S_N}2\) mechanism. The rate of the \(\mathrm{S_N}1\) mechanism is independent of the nature of the nucleophile. The nucleophile does not react in the slow step of \(\mathrm{S_N}1\); it waits till the carbocation intermediate is formed, and then reacts fast with it. A stronger nucleophile therefore cannot speed up something it is not part of.

Three working rules help you compare nucleophiles. First, a negatively charged nucleophile is more powerful than its conjugate acid; for example, \(\mathrm{R\!-\!O^-}\) is a better nucleophile than \(\mathrm{R\!-\!OH}\), because the full negative charge holds a more available electron pair. Second, when the donor atoms are from the same period of the periodic table, nucleophilicity decreases from left to right in a period; for example, \(\mathrm{H_2O}\) is a less powerful nucleophile than \(\mathrm{NH_3}\), since the more electronegative oxygen holds its lone pairs more tightly. Third, when the donor atoms are from the same group of the periodic table, nucleophilicity increases down the group; for example, \(\mathrm{I^-}\) is a better nucleophile than \(\mathrm{Cl^-}\), because the larger, more loosely held electron cloud of iodide is more easily offered to carbon.

nucleophilic strength (Across a period →: nucleophilicity decreases, e.g. \(\mathrm{NH_3} > \mathrm{H_2O}\), because increasing electronegativity holds the lone pair more tightly. Down a group ↓: nucleophilicity increases, e.g. \(\mathrm{I^-} > \mathrm{Br^-} > \mathrm{Cl^-}\), because the larger ion is more polarisable and its electrons are more loosely held. Charge: the anion always beats its conjugate acid, \(\mathrm{RO^-} > \mathrm{ROH}\). A stronger nucleophile speeds up \(\mathrm{S_N}2\) only — \(\mathrm{S_N}1\) is indifferent to it.)

c. Solvent Polarity

The \(\mathrm{S_N}1\) mechanism proceeds via the formation of a carbocation intermediate. A good ionizing solvent, that is, a polar solvent, stabilizes the ions by solvation — surrounding each ion with a shell of solvent molecules oriented towards its charge. Solvation of the carbocation is relatively poor, and solvation of the anion is particularly important. Anions are solvated by hydrogen bonding solvents, that is, protic solvents such as water and alcohols. Thus the \(\mathrm{S_N}1\) reaction proceeds more rapidly in polar protic solvents than in aprotic solvents.

Polar protic solvents usually decrease the rate of the \(\mathrm{S_N}2\) reaction. In the rate determining step of the \(\mathrm{S_N}2\) mechanism, the substrate as well as the nucleophile is involved. A polar solvent stabilizes the nucleophile, one of the reactants, by solvation. Thus the solvent deactivates the nucleophile by stabilizing it — wrapping it in a cage of solvent molecules that must be stripped away before it can attack. Hence aprotic solvents, or solvents of low polarity, will favour the \(\mathrm{S_N}2\) mechanism.

Which of the following two compounds would react faster by the \(\mathrm{S_N}2\) mechanism and why?

\[\mathrm{CH_3\!-\!CH_2\!-\!CH_2\!-\!CH_2Cl} \qquad \mathrm{CH_3\!-\!CHCl\!-\!CH_2\!-\!CH_3}\]

\[\text{1-Chlorobutane} \qquad\qquad \text{2-Chlorobutane}\]

In the \(\mathrm{S_N}2\) mechanism, a pentacoordinate T.S. is involved. The order of reactivity of alkyl halides towards the \(\mathrm{S_N}2\) mechanism is Primary > Secondary > Tertiary, due to increasing crowding in the T.S. from primary to tertiary halides. 1-Chlorobutane, being a primary halide, will react faster by the \(\mathrm{S_N}2\) mechanism than the secondary halide 2-chlorobutane.

Predict which mechanism, \(\mathrm{S_N}1\) or \(\mathrm{S_N}2\), each of the following reactions will follow, and state what you would observe about the optical activity of the product.

(i) \(\mathrm{CH_3\!-\!CH_2\!-\!CH_2\!-\!Br}\) warmed with \(\mathrm{KOH}\) in acetone.

(ii) Optically active 2-bromo-2-methylbutane warmed with aqueous \(\mathrm{KOH}\).

  1. The substrate is a primary halide, so the crowding in the pentacoordinate transition state is least here, and \(\mathrm{S_N}2\) is favoured. Acetone is an aprotic solvent, which leaves the hydroxide ion poorly solvated and therefore highly reactive — again favouring \(\mathrm{S_N}2\). Both factors point the same way, so the reaction follows the \(\mathrm{S_N}2\) mechanism. The reacting carbon here is not chiral, since it carries two hydrogen atoms, so no question of optical rotation arises for the product.

  2. The substrate is a tertiary halide. A tertiary carbocation is well stabilized by the \(+\mathrm{I}\) effect and hyperconjugation of three alkyl groups, and its formation also relieves the crowding in the substrate. Water is a polar protic solvent, which stabilizes both the carbocation and the departing bromide ion. Hence the reaction follows the \(\mathrm{S_N}1\) mechanism. Since the reacting carbon is chiral, the planar carbocation can be attacked from either face, so the product is obtained as a nearly racemic mixture and is very nearly optically inactive.

(i) Arrange the following in decreasing order of reactivity towards the \(\mathrm{S_N}2\) mechanism: 2-bromo-2-methylpropane, 1-bromopropane, 2-bromopropane, bromomethane. (ii) Which of \(\mathrm{CH_3CH_2Cl}\) and \(\mathrm{CH_3CH_2I}\) would you expect to undergo nucleophilic substitution faster, and why? (iii) Name the mechanism by which 3-chloro-3-methylpentane would react with aqueous \(\mathrm{NaOH}\), and state whether the product would be optically active.

• How are alkenes prepared from alkyl halides? • Which is the stronger base from the following? i. aq. \(\mathrm{KOH}\) ii. alc. \(\mathrm{KOH}\)

10.6.5 Elimination Reaction : Dehydrohalogenation

When an alkyl halide having at least one \(\beta\)-hydrogen is boiled with an alcoholic solution of potassium hydroxide, it undergoes elimination of a hydrogen atom from the \(\beta\)-carbon and a halogen atom from the \(\alpha\)-carbon, resulting in the formation of an alkene.

Before going further, fix the labels firmly. The carbon bearing the halogen is commonly called the \(\alpha\)-carbon (alpha carbon), and any carbon attached to the \(\alpha\)-carbon is a \(\beta\)-carbon (beta carbon). Hydrogens attached to a \(\beta\)-carbon are \(\beta\)-hydrogens. An alkyl halide with no \(\beta\)-hydrogen at all simply cannot undergo this reaction.

This reaction is called a \(\beta\)-elimination (or 1,2-elimination) reaction, as it involves elimination of the halogen and a \(\beta\)-hydrogen atom from adjacent carbons, as drawn in Fig. 10.25.

Diagram

Fig. 10.25 – General β-elimination: a base B: with its lone pair shown attacking a β-hydrogen of the fragment H–Cβ–Cα(X)–, with curly arrows for the removal of the β-hydrogen, formation of the C=C π bond and departure of X⁻; over the arrow write alc. KOH, Δ; products drawn as the alkene C=C, B⁺H and X⁻; label base, alkyl halide and alkene.

NoteDefinition

\(\beta\)-elimination is the removal of a halogen atom from the \(\alpha\)-carbon and a hydrogen atom from an adjacent \(\beta\)-carbon of an alkyl halide, giving an alkene.

As hydrogen and halogen are removed in this reaction, it is also known as a dehydrohalogenation reaction.

If there are two or more non-equivalent \(\beta\)-hydrogen atoms in a halide, then this reaction gives a mixture of products. Thus, 2-bromobutane on heating with alcoholic \(\mathrm{KOH}\) gives a mixture of but-1-ene and but-2-ene. Writing the substrate as \(\mathrm{CH_3\!-\!CH_2\!-\!CHBr\!-\!CH_3}\), the \(\alpha\)-carbon is the one carrying bromine; the \(\mathrm{CH_2}\) on its left is one \(\beta\)-carbon, labelled \(\beta^1\), and the terminal \(\mathrm{CH_3}\) on its right is the other, labelled \(\beta^2\). The two possible eliminations are shown in Fig. 10.26.

Loss of a \(\beta^2\)-hydrogen, from the terminal methyl group, places the double bond at the end of the chain and gives but-1-ene, \(\mathrm{CH_3\!-\!CH_2\!-\!CH{=}CH_2}\). Loss of a \(\beta^1\)-hydrogen, from the \(\mathrm{CH_2}\) group, places the double bond in the middle of the chain and gives but-2-ene, \(\mathrm{CH_3\!-\!CH{=}CH\!-\!CH_3}\).

Flowchart

FC 10.6 – Dehydrohalogenation of 2-bromobutane: CH₃–CH₂–CHBr–CH₃ + alc. KOH, Δ → branch 1: loss of β²-hydrogen (from the terminal CH₃) → CH₃–CH₂–CH=CH₂, but-1-ene (minor); branch 2: loss of β¹-hydrogen (from the CH₂) → CH₃–CH=CH–CH₃, but-2-ene (major, by Saytzeff rule).

Diagram

Fig. 10.26 – 2-Bromobutane drawn as CH₃–CH₂–CH(Br)–CH₃ with the α-carbon and the two β-carbons labelled β¹ and β², and two downward arrows from it marked alc. KOH, Δ: the left arrow labelled “loss of β²-hydrogen” leading to CH₃–CH₂–CH=CH₂ (But-1-ene) and the right arrow labelled “loss of β¹-hydrogen” leading to CH₃–CH=CH–CH₃ (But-2-ene).

The different products of elimination do not form in equal proportion. After studying a number of elimination reactions, the Russian chemist Saytzeff formulated an empirical rule, given below.

NotePrinciple / Law

Saytzeff’s rule: in a dehydrohalogenation reaction, the preferred product is that alkene which has the greater number of alkyl groups attached to the doubly bonded carbon atoms.

Therefore, in the above reaction but-2-ene is the preferred product, and is formed as the major product. Count the alkyl groups to check this: but-2-ene has a methyl group on each of the two doubly bonded carbons, while but-1-ene has one ethyl group on one of them and nothing on the other.

It turned out that more highly substituted alkenes are also more stable alkenes. Hence Saytzeff elimination is the preferred formation of the more highly stabilized alkene during an elimination reaction. The stability order of alkyl substituted alkenes is:

\[\mathrm{R_2C{=}CR_2} > \mathrm{R_2C{=}CHR} > \mathrm{R_2C{=}CH_2},\ \mathrm{RCH{=}CHR} > \mathrm{RCH{=}CH_2}\]

The rule is named after Alexander Saytzeff, who taught at Kazan in Russia in the 1870s and arrived at it purely by collecting the results of many elimination experiments and looking for the pattern. It is worth noticing that he had no theory of alkene stability to guide him — that explanation came later. An empirical rule that survives long enough usually turns out to have a reason hiding behind it.

2-Bromo-2-methylbutane is heated with alcoholic \(\mathrm{KOH}\). Write the structures of all the alkenes formed and identify the major product.

The substrate is \(\mathrm{CH_3\!-\!CBr(CH_3)\!-\!CH_2\!-\!CH_3}\). The \(\alpha\)-carbon is the one bearing bromine. It has three \(\beta\)-carbons: the two methyl groups attached to it, and the \(\mathrm{CH_2}\) of the ethyl group.

Removing a hydrogen from either methyl group and the bromine from the \(\alpha\)-carbon places the double bond between the \(\alpha\)-carbon and that methyl carbon, giving 2-methylbut-1-ene:

\[\mathrm{CH_2{=}C(CH_3)\!-\!CH_2\!-\!CH_3}\]

Removing a hydrogen from the \(\mathrm{CH_2}\) group instead places the double bond between the \(\alpha\)-carbon and that carbon, giving 2-methylbut-2-ene:

\[\mathrm{CH_3\!-\!C(CH_3){=}CH\!-\!CH_3}\]

Now apply Saytzeff’s rule. In 2-methylbut-1-ene the doubly bonded carbons carry two alkyl groups between them; in 2-methylbut-2-ene they carry three. The more highly substituted alkene is the more stable one, so 2-methylbut-2-ene is the major product and 2-methylbut-1-ene the minor product.

Elimination versus Substitution

Alkyl halides undergo substitution as well as elimination reactions. Both reactions are brought about by a basic reagent, hence there is always a competition between these two reactions. The same species can pull a proton off the \(\beta\)-carbon, giving elimination, or attack the \(\alpha\)-carbon, giving substitution. The reaction which actually predominates depends upon the following factors.

a. Nature of alkyl halides : Tertiary alkyl halides prefer to undergo elimination reaction, whereas primary alkyl halides prefer to undergo substitution reaction.

b. Strength and size of nucleophile : A bulkier electron rich species prefers to act as a base by abstracting a proton, and thus favours elimination — a large species finds a \(\beta\)-hydrogen on the outside of the molecule easier to reach than the crowded carbon within. Substitution is favoured in the case of comparatively weaker bases, which prefer to act as nucleophiles.

c. Reaction conditions : A less polar solvent and a high temperature favour elimination, whereas a low temperature and a polar solvent favour substitution reaction.

aqueous \(\mathrm{KOH}\) versus alcoholic \(\mathrm{KOH}\) (The same alkali, two different outcomes → in water, the hydroxide ion is heavily hydrogen-bonded to the solvent and acts mainly as a nucleophile, attacking the \(\alpha\)-carbon → use aqueous \(\mathrm{KOH}\) when you want the alcohol. In alcohol the medium provides alkoxide ions, which are stronger and bulkier bases and prefer to abstract a \(\beta\)-hydrogen → use alcoholic \(\mathrm{KOH}\), with boiling, when you want the alkene. This single pair of conditions is the most frequently examined reagent contrast in the whole chapter.)

nucleophilic substitution vs elimination

Factor Favours substitution Favours elimination
Nature of the alkyl halide Primary Tertiary
Reagent Weaker base acting as a nucleophile Stronger, bulkier base
Solvent Polar Less polar
Temperature Low High
Typical conditions aq. \(\mathrm{KOH}\) alc. \(\mathrm{KOH}\), boiling
Product Alcohol (or other substituted product) Alkene
Bond changes at carbon \(\mathrm{C\!-\!X}\) replaced by \(\mathrm{C\!-\!Nu}\) \(\mathrm{C\!-\!X}\) and \(\mathrm{C\!-\!H}\) both lost, \(\mathrm{C{=}C}\) formed

(i) Write the structures of all the alkenes obtained when 2-bromopentane is heated with alcoholic \(\mathrm{KOH}\), and name the major product. (ii) Why does 2,2-dimethyl-1-chloropropane fail to give any alkene with alcoholic \(\mathrm{KOH}\)? (iii) An alkyl halide is treated with \(\mathrm{KOH}\); in one experiment the product is an alcohol and in another it is an alkene. State the two sets of conditions used.

How This Is Tested

This section supplies more examination questions than any other in the chapter. Expect: distinguish between \(\mathrm{S_N}1\) and \(\mathrm{S_N}2\) mechanisms (a standard long-answer question); choose the compound that reacts fastest by a stated mechanism; identify which compound undergoes racemization during alkaline hydrolysis; predict the major product of dehydrohalogenation using Saytzeff’s rule; and complete a conversion in which the reagent must be chosen to give substitution rather than elimination. Two habits protect you here. First, always classify the substrate as \(1^\circ\), \(2^\circ\) or \(3^\circ\) before anything else. Second, read the solvent and the temperature, because they, and not the alkali alone, often decide the answer.

The silver halide test of section 10.6.1 is the everyday working method for detecting halogen in an unknown organic compound, and it is the reason a qualitative analysis bench always carries a bottle of silver nitrate. Two practical cautions go with it. Silver nitrate solution stains skin and clothing a stubborn black, because the silver ion is reduced to metallic silver by light and by the substances on your skin, so it should be handled with care and washed off immediately. And the order of addition matters: the alkaline mixture must be acidified with dilute nitric acid before the silver nitrate is added, or a brown precipitate of silver oxide will form and be mistaken for a positive result. The reactions of Table 10.3, meanwhile, are not merely classroom exercises — converting an alkyl halide into a nitrile and then into a carboxylic acid or an amine is one of the standard ways of lengthening a carbon chain by one atom, and this strategy is used routinely in the synthesis of medicines and fine chemicals.

10.7 Uses and Environmental Effects of Some Polyhalogen Compounds

Compounds carrying more than one halogen atom occupy an uncomfortable place in chemistry. The very properties that make them useful — chemical stability, low flammability, an ability to dissolve oils and greases — are the properties that make them persist in the body and in the environment long after their work is done. The six compounds in this section are studied together for exactly this reason: each has a genuine use, and each carries a cost. Their structures are drawn in Fig. 10.36.

Diagram

Fig. 10.36 – Structural formulae of five polyhalogen compounds drawn side by side with names below each: CH₂Cl₂ (dichloromethane), CHCl₃ (chloroform), CCl₄ (carbon tetrachloride), CHI₃ (iodoform) and CCl₂F₂ (Freon-12); show all bonds from the central carbon.

10.7.1 Dichloromethane / Methylene Chloride (\(\mathrm{CH_2Cl_2}\))

It is a colourless volatile liquid with a moderately sweet aroma. It is used as a solvent, and used as a propellant in aerosols.

Over exposure to dichloromethane causes dizziness, fatigue, nausea, headaches, numbness and weakness. It is highly dangerous if it comes in direct contact with the eyes, as it damages the cornea.

Its volatility is what makes it useful and dangerous at the same time: a liquid that evaporates readily leaves a work surface quickly, but it also fills the air of a closed room quickly.

10.7.2 Chloroform / Trichloromethane (\(\mathrm{CHCl_3}\))

It is a colourless liquid with a peculiar sweet smell. It is used to prepare chlorofluoromethane, a refrigerant R-22. It is used as a solvent for the extraction of natural products like gums, fats and resins. It is also used as a source of dichlorocarbene.

Chloroform causes depression of the central nervous system. Inhaling chloroform for a short time causes fatigue, dizziness and headache. Long exposure to chloroform may affect the liver.

Chloroform, when exposed to air and light, forms a poisonous compound phosgene, so it is stored in dark coloured air tight bottles. The dark glass keeps out the light and the tight stopper keeps out the air; remove either precaution and the bottle slowly manufactures its own poison.

chloroform, \(\mathrm{CHCl_3}\) (Serves as a source of the reactive species dichlorocarbene → requires treatment with a strong base such as alcoholic \(\mathrm{KOH}\) → used in synthesis where a \(\mathrm{CCl_2}\) fragment has to be delivered to a molecule, and as a solvent for extracting gums, fats and resins; must be stored in dark, air-tight bottles because light and air convert it into phosgene.)

10.7.3 Carbon Tetrachloride / Tetrachloromethane (\(\mathrm{CCl_4}\))

It is a colourless liquid with a sweet smell. It is a very useful solvent for oils, fats and resins. It serves as a source of chlorine. It is used as a cleaning agent.

It is highly toxic to the liver. Exposure to a high concentration of \(\mathrm{CCl_4}\) can affect the central nervous system, and it is suspected to be carcinogenic. Prolonged exposure may cause death. It is also a greenhouse gas.

Q. Why do these solvents dissolve oils, fats and resins so readily when they will not dissolve in water at all?

A. Because of the rule you met in section 10.4.3 — like dissolves like. Oils, fats and resins are large, essentially non-polar molecules held together by weak van der Waals forces, and a polyhalogen compound can slip between them and set up the same kind of weak attractions. Water cannot, because its molecules would have to break their own hydrogen bonds and would gain nothing in return. The same structural fact therefore explains both the industrial usefulness of these liquids and their refusal to mix with water.

10.7.4 Iodoform or Triiodomethane (\(\mathrm{CHI_3}\))

It is a yellow crystalline substance with a disagreeable smell. It is used in medicine as a healing agent and antiseptic in the dressing of wounds; however, its use is limited.

It causes irritation to the skin and eyes. It may cause respiratory irritation or breathing difficulty, dizziness, nausea, depression of the central nervous system and visual disturbance.

10.7.5 Freons

These are organic compounds of chlorine and fluorine — chlorofluorocarbons, CFCs — commonly used as refrigerants. The most common representative is dichlorodifluoromethane (Freon-12); others include chlorodifluoromethane (R-22) and trichlorofluoromethane (R-11), and so on.

They are used as refrigerants in fridges and air conditioning, as propellants in aerosols, and as solvents. They are used as blowing agents in making foams and packing materials.

Chlorofluorocarbons are responsible for ozone depletion in the stratosphere. Regular large inhalation of freons results in breathing problems, organ damage and loss of consciousness.

How CFCs Destroy the Ozone Layer

When ultraviolet radiation (UV) strikes a CFC molecule such as \(\mathrm{CFCl_3}\) in the upper atmosphere, the carbon–chlorine bond breaks and produces a highly reactive chlorine atom.

\[\mathrm{CFCl_3} \rightarrow \mathrm{CFCl_2} + \mathrm{Cl}\]

This reactive chlorine atom decomposes an ozone molecule (\(\mathrm{O_3}\)) into an oxygen molecule (\(\mathrm{O_2}\)).

\[\mathrm{O_3} + \mathrm{Cl} \rightarrow \mathrm{O_2} + \mathrm{ClO}\]

\[\mathrm{ClO} + \mathrm{O} \rightarrow \mathrm{O_2} + \mathrm{Cl}\]

One atom of chlorine can destroy up to 100,000 ozone molecules. The sequence is set out as a cycle in FC 10.9.

Flowchart

FC 10.9 – Catalytic destruction of ozone by chlorine: CFCl₃ + UV radiation → CFCl₂ + Cl atom → Cl attacks O₃ → O₂ + ClO → ClO meets an O atom → O₂ + Cl atom regenerated → the regenerated Cl atom returns to attack another O₃ molecule, closing the cycle; note beside the cycle that one Cl atom can destroy up to 100,000 O₃ molecules.

Q. Why can a single chlorine atom destroy such an enormous number of ozone molecules?

A. Look carefully at the last equation. The chlorine atom that was used up in the first step reappears at the end of the second step, unchanged and ready to attack again. It is therefore acting as a catalyst — taking part in the reaction, speeding up the destruction of ozone, and emerging from it intact. Nothing removes it from the cycle, so a single atom keeps working its way through ozone molecule after ozone molecule until some other process finally traps it.

You met the origin of this problem in the story that opened this chapter, where a refrigerant designed to be harmless proved harmless only at ground level. The chemistry above is the reason why: the same unreactivity that keeps a CFC safe in a kitchen also keeps it intact all the way up to the stratosphere, where ultraviolet radiation strong enough to break the C–Cl bond is waiting.

Diagram

Fig. 10.37 – A schematic dual-trend graph with time in decades along the x-axis: one curve showing atmospheric CFC concentration rising steeply from the mid-twentieth century, flattening near the end of the 1980s and slowly declining afterwards; a second curve showing stratospheric ozone over Antarctica falling as the first curve rises and beginning to recover late; label both axes and mark the point where international restrictions on CFC production began.

the CFC and ozone trends of Fig. 10.37 (Study the two curves and answer: (a) Describe in one sentence how the ozone curve responds to the CFC curve. (b) The CFC curve flattens some years before the ozone curve begins to recover — suggest, using the chemistry of FC 10.9, why the improvement is delayed rather than immediate. (c) Would you expect the recovery of ozone to be faster or slower than the original depletion, and why? (d) What does the shape of these curves suggest about the wisdom of testing a new refrigerant only for its behaviour at ground level?)

10.7.6 Dichlorodiphenyltrichloroethane (DDT)

It is a colourless, tasteless and odourless crystalline compound having insecticidal property. Its structure is shown in Fig. 10.38 — two chlorine-substituted benzene rings joined to a carbon that also carries a trichloromethyl group.

It kills insects such as houseflies, mosquitoes and body lice. It was used for controlling malaria and typhus.

Diagram

Fig. 10.38 – Structure of DDT: a central carbon bonded to a CCl₃ group above it and to two benzene rings, each ring carrying a Cl atom at the para position; label the CCl₃ group and the two para chlorine atoms.

Exposure to high doses of DDT may cause vomiting, tremors or shakiness. Laboratory animal studies showed adverse effects of DDT on the liver and reproduction.

DDT is a persistent organic pollutant, readily absorbed in soils, and it tends to accumulate in the ecosystem. When dissolved in oil or another liquid, it is readily absorbed by the skin. It is resistant to metabolism. It accumulates in fatty tissues. There is a ban on the use of DDT due to all these adverse effects.

NoteDefinition

A persistent organic pollutant is a substance that resists breakdown in the environment, spreads widely from where it was released, and builds up in the tissues of living organisms.

Q. Why does DDT settle in fatty tissue instead of being flushed out of the body?

A. Because of its solubility, once again. DDT is a large, essentially non-polar molecule; it cannot form hydrogen bonds with water and so is not carried away in urine, but it dissolves readily in fats and oils. Any DDT that enters an animal therefore migrates into fatty tissue and stays there. Since the compound is also resistant to metabolism, the body has no efficient way of breaking it down, so each fresh exposure adds to the store already present.

DDT, the first of the chlorinated organic insecticides, was originally prepared in 1873, but it was not until 1939 that Paul Muller of Geigy Pharmaceuticals in Switzerland discovered the effectiveness of DDT as an insecticide. Muller was awarded the Nobel Prize in Medicine and Physiology in 1948 for this discovery. The use of DDT increased enormously on a worldwide basis after World War II, primarily because of its effectiveness against the mosquito that spreads malaria and the lice that carry typhus. In time, many species of insects developed resistance to DDT, and it was also discovered to have a high toxicity towards fish. DDT is not metabolised very rapidly by animals; instead, it is deposited and stored in fatty tissues. Public concern grew after Rachel Carson’s book Silent Spring appeared in 1962, and the use of DDT was banned in the United States in 1973, although it is still in use in some other parts of the world.

the polyhalogen compounds of this section

Compound Formula Appearance Principal uses Chief hazard
Dichloromethane \(\mathrm{CH_2Cl_2}\) Colourless volatile liquid, moderately sweet aroma Solvent; aerosol propellant Dizziness, nausea, numbness; damages the cornea
Chloroform \(\mathrm{CHCl_3}\) Colourless liquid, peculiar sweet smell Preparing R-22; solvent for gums, fats, resins; source of dichlorocarbene Depresses the central nervous system; affects the liver; forms phosgene in air and light
Carbon tetrachloride \(\mathrm{CCl_4}\) Colourless liquid, sweet smell Solvent for oils, fats, resins; source of chlorine; cleaning agent Highly toxic to the liver; suspected carcinogen; greenhouse gas
Iodoform \(\mathrm{CHI_3}\) Yellow crystalline solid, disagreeable smell Antiseptic and healing agent in dressings (limited use) Irritates skin and eyes; respiratory and nervous effects
Freons (CFCs) e.g. \(\mathrm{CCl_2F_2}\) Volatile gases or low-boiling liquids Refrigerants; aerosol propellants; solvents; foam blowing agents Deplete stratospheric ozone; inhalation causes organ damage
DDT — Colourless, tasteless, odourless crystalline solid Insecticide against houseflies, mosquitoes, body lice Persistent organic pollutant; accumulates in fatty tissue; toxic to fish

Chloroform has the molecular formula \(\mathrm{CHCl_3}\). (i) Calculate the mass percentage of chlorine in chloroform. (ii) How many moles of chlorine atoms are present in 23.9 g of chloroform? (Atomic masses: \(\mathrm{C} = 12\), \(\mathrm{H} = 1\), \(\mathrm{Cl} = 35.5\))

  1. First find the molar mass of chloroform by adding the atomic masses of all its atoms.

\[M(\mathrm{CHCl_3}) = 12 + 1 + (3 \times 35.5) = 12 + 1 + 106.5 = 119.5\ \text{g mol}^{-1}\]

Of this, the mass contributed by chlorine is \(106.5\ \text{g mol}^{-1}\).

\[\%\ \mathrm{Cl} = \frac{106.5}{119.5} \times 100 = 89.12\ \%\]

Nearly nine-tenths of the mass of chloroform is chlorine — which is why polyhalogen compounds are so much denser than the hydrocarbons they come from.

  1. The number of moles of chloroform in 23.9 g is

\[n = \frac{23.9\ \text{g}}{119.5\ \text{g mol}^{-1}} = 0.200\ \text{mol}\]

Each molecule of \(\mathrm{CHCl_3}\) contains three chlorine atoms, so

\[n(\mathrm{Cl}) = 3 \times 0.200 = 0.600\ \text{mol}\]

There are 0.600 mol of chlorine atoms in the sample.

(i) Calculate the mass percentage of chlorine in carbon tetrachloride (\(\mathrm{C} = 12\), \(\mathrm{Cl} = 35.5\)). (ii) Write the two equations by which a chlorine atom destroys ozone, and explain why the chlorine atom is described as a catalyst. (iii) Give one reason each for the following: chloroform is stored in dark air-tight bottles; DDT accumulates in the fatty tissue of fish; carbon tetrachloride is classified as a greenhouse gas.

The story of these compounds has changed how chemists choose a solvent. Carbon tetrachloride was once poured into hand-held fire extinguishers and used freely for cleaning; both practices were abandoned when its toxicity became clear and when it was found that hot surfaces convert it into phosgene, so that the extinguisher could be more dangerous than the fire. Chlorinated solvents that were once standard in teaching laboratories have been steadily replaced by less hazardous liquids, and where a chlorinated solvent is genuinely necessary the modern practice is to use the smallest quantity possible, in a fume cupboard, with the vapour recovered rather than vented. This is the practical face of green chemistry: not a slogan about the environment, but a sequence of specific decisions — choose a safer solvent, use less of it, contain the vapour, recover what you can. When you next see a procedure that specifies dichloromethane, it is worth asking the question a working chemist now asks routinely: is there something safer that would do the same job?

How This Is Tested

Questions on this section are short and factual, and they nearly always pair a use with a hazard: “give two uses of chloroform and state why it is stored in dark bottles”, “which compound is used as a source of dichlorocarbene”, “why is DDT called a persistent organic pollutant”. The CFC–ozone equations are asked as a three-mark item requiring both steps and the conclusion that chlorine is regenerated. Assertion–reason questions often use the pairing “CFCs are chemically unreactive” with “CFCs are harmless to the environment”, where the assertion is true but the reason is false — and the explanation for that mismatch is the whole content of section 10.7.5.

10.8 Summary

  1. Replacing one or more hydrogen atoms of an aliphatic or aromatic hydrocarbon by halogen atoms gives a halogen derivative, written in general as \(\mathrm{R\!-\!X}\) where \(\mathrm{X} = \mathrm{F}\), \(\mathrm{Cl}\), \(\mathrm{Br}\) or \(\mathrm{I}\).

  2. On the basis of the carbon skeleton they are classified as haloalkanes, haloalkenes, haloalkynes and haloarenes; on the basis of the number of halogen atoms as mono, di, tri or poly halogen compounds.

  3. Monohalogen compounds are classified further by the position of the halogen and the hybridization of the carbon carrying it: alkyl (sp³), allylic (sp³, next to C=C), benzylic (sp³, attached to a ring), vinylic (sp²), haloalkyne (sp) and aryl (sp², on the ring).

  4. Alkyl halides are primary, secondary or tertiary according to the number of carbon atoms attached to the carbon that bears the halogen. This label decides much of the chemistry that follows.

  5. Common names take the alkyl group followed by the halide: ethyl bromide, tert-butyl chloride. IUPAC names treat the halogen only as a prefix — fluoro, chloro, bromo, iodo — before the parent alkane name, so the same compound is bromoethane.

  6. For dihalogen derivatives of an arene, the common system uses o-, m-, p- while the IUPAC system uses 1,2- ; 1,3- and 1,4-.

  7. When a multiple bond is present it takes the lower locant, even if that pushes the halogen to a higher number.

  8. From alcohols, using a halogen acid: \(\mathrm{R\!-\!OH} + \mathrm{HX} \rightarrow \mathrm{R\!-\!X} + \mathrm{H_2O}\). The reactivity order of alcohols is \(3^\circ > 2^\circ > 1^\circ\). Primary and secondary alcohols need anhydrous \(\mathrm{ZnCl_2}\) with \(\mathrm{HCl}\) (Grooves’ process); concentrated \(\mathrm{HCl}\) with anhydrous \(\mathrm{ZnCl_2}\) is Lucas reagent.

  9. \(\mathrm{HBr}\) is generated in situ from \(\mathrm{NaBr}\) and \(\mathrm{H_2SO_4}\); \(\mathrm{HI}\) from \(\mathrm{NaI}\) in 95% phosphoric acid.

  10. From alcohols, using a phosphorus halide: \(3\,\mathrm{R\!-\!OH} + \mathrm{PX_3} \rightarrow 3\,\mathrm{R\!-\!X} + \mathrm{H_3PO_3}\) and \(\mathrm{R\!-\!OH} + \mathrm{PCl_5} \rightarrow \mathrm{R\!-\!Cl} + \mathrm{HCl} + \mathrm{POCl_3}\). These minimise rearrangement of the carbon skeleton.

  11. From alcohols, using thionyl chloride: \(\mathrm{R\!-\!OH} + \mathrm{SOCl_2} \xrightarrow{\ \Delta\ } \mathrm{R\!-\!Cl} + \mathrm{SO_2}\uparrow + \mathrm{HCl}\uparrow\). Both by-products are gases, so no separation is needed and the method is preferred for alkyl chlorides.

  12. From hydrocarbons: halogenation of alkanes is unsuitable because a mixture of mono and poly halogen compounds forms. Addition of \(\mathrm{HX}\) to an alkene follows Markownikov’s rule, and \(\mathrm{HBr}\) in the presence of peroxide adds the other way round (peroxide effect). Alkenes with \(\mathrm{Cl_2}\) or \(\mathrm{Br_2}\) in \(\mathrm{CCl_4}\) at room temperature give vicinal dihalides, while at high temperature the allylic hydrogen is substituted instead.

  13. Halogen exchange: \(\mathrm{R\!-\!Cl} + \mathrm{NaI} \xrightarrow{\ \text{acetone}\ } \mathrm{R\!-\!I} + \mathrm{NaCl}\downarrow\) is the Finkelstein reaction; \(\mathrm{R\!-\!Cl} + \mathrm{AgF} \rightarrow \mathrm{R\!-\!F} + \mathrm{AgCl}\downarrow\) is the Swartz reaction.

  14. Aryl halides are prepared by electrophilic halogenation of benzene and its derivatives, in the dark with a Lewis acid catalyst (\(\mathrm{Fe}\), \(\mathrm{FeCl_3}\), anhydrous \(\mathrm{AlCl_3}\)), or from diazonium salts by Sandmeyer’s reaction. Iodination is reversible and needs \(\mathrm{HNO_3/HIO_4}\) to remove \(\mathrm{HI}\); fluorination is too violent to use.

  15. The \(\mathrm{C\!-\!X}\) bond is polar covalent: carbon carries \(\delta+\) and halogen \(\delta-\), which makes the carbon the point of attack for nucleophiles.

  16. From \(\mathrm{F}\) to \(\mathrm{I}\) the bond length increases and the bond enthalpy decreases, because the halogen p-orbital becomes more diffuse and overlaps the carbon orbital less well.

  17. Boiling points are higher than those of the corresponding alkanes, and follow \(\mathrm{RI} > \mathrm{RBr} > \mathrm{RCl} > \mathrm{RF}\). They rise with chain length and fall with branching, since branching reduces surface area and weakens van der Waals forces.

  18. Alkyl halides and aryl halides are insoluble in water, because they cannot form hydrogen bonds with it, but dissolve in non-polar organic solvents.

  19. Isomeric dihalobenzenes have nearly the same boiling points, but the para isomer melts much higher because its symmetrical structure packs closely in the crystal lattice.

  20. A carbon carrying four different groups is a chiral carbon, marked with an asterisk. A molecule with one chiral carbon is chiral: it is not superimposable on its mirror image, just as a left hand is not superimposable on a right.

  21. Plane polarized light has oscillations in only one plane and is obtained by passing ordinary light through a Nicol’s prism.

  22. Optical activity is the rotation of the plane of polarization by a substance, measured as the optical rotation. Rotation to the right is dextrorotatory, d- or (+); to the left is laevorotatory, l- or (−).

  23. Non-superimposable mirror images are enantiomers. They have identical physical properties except for the sign of optical rotation, and identical chemical properties except towards optically active reagents.

  24. An equimolar mixture of two enantiomers is a racemic modification, (dl) or (±), and is optically inactive because the two rotations cancel.

  25. Configuration is shown on paper by the wedge formula (bold wedge above the plane, broken wedge below) or by the Fischer projection, in which horizontal bonds lie above the plane and vertical bonds below.

  26. Laboratory test: warming with aqueous alkali gives the halide ion, \(\mathrm{R\!-\!X} + \mathrm{OH^-} \xrightarrow{\ \Delta\ } \mathrm{R\!-\!OH} + \mathrm{X^-}\); acidifying with dilute \(\mathrm{HNO_3}\) and adding \(\mathrm{AgNO_3}\) then precipitates silver halide, \(\mathrm{Ag^+} + \mathrm{X^-} \rightarrow \mathrm{AgX}\downarrow\).

  27. The C–X carbon is an electrophilic centre, so haloalkanes undergo nucleophilic substitution (\(\mathrm{S_N}\)) with a wide range of nucleophiles, giving alcohols, ethers, esters, amines, nitriles, isocyanides, alkyl nitrites and nitroalkanes.

  28. Cyanide and nitrite are ambident nucleophiles: \(\mathrm{KCN}\) gives mainly the cyanide (nitrile) and \(\mathrm{AgCN}\) the isocyanide; \(\mathrm{KNO_2}\) gives the alkyl nitrite and \(\mathrm{AgNO_2}\) the nitroalkane.

  29. Reactivity in \(\mathrm{S_N}\) reactions increases with substitution state, \(3^\circ > 2^\circ > 1^\circ\), and with the halogen in the order \(\mathrm{R\!-\!I} > \mathrm{R\!-\!Br} > \mathrm{R\!-\!Cl}\). The halogen that leaves with the bond pair is the leaving group.

  30. \(\mathrm{S_N}2\) is a single step reaction in which bond breaking and bond forming happen together. The nucleophile attacks from the side opposite the leaving group, the transition state has a pentacoordinate carbon, and the product has the opposite configuration — inversion, known as Walden inversion.

  31. \(\mathrm{S_N}1\) is a two step reaction: slow, reversible heterolysis of the C–X bond gives a planar carbocation, which is then attacked rapidly by the nucleophile. Because attack can occur from either face, the product is largely racemic.

  32. \(\mathrm{S_N}2\) is favoured by primary halides and \(\mathrm{S_N}1\) by tertiary halides; secondary halides may follow either route. Allylic and benzylic halides react well by \(\mathrm{S_N}1\) because their carbocations are resonance stabilised.

  33. A stronger nucleophile favours \(\mathrm{S_N}2\); the rate of \(\mathrm{S_N}1\) does not depend on the nucleophile at all. Polar protic solvents favour \(\mathrm{S_N}1\) by solvating the ions, while aprotic or less polar solvents favour \(\mathrm{S_N}2\) because they leave the nucleophile free.

  34. Elimination: boiling an alkyl halide having at least one \(\beta\)-hydrogen with alcoholic \(\mathrm{KOH}\) removes a hydrogen from the \(\beta\)-carbon and the halogen from the \(\alpha\)-carbon to give an alkene. This \(\beta\)-elimination is also called dehydrohalogenation.

  35. Where two or more non-equivalent \(\beta\)-hydrogens are available, a mixture forms and Saytzeff’s rule applies: the preferred product is the alkene with the greater number of alkyl groups on the doubly bonded carbons, which is also the more stable alkene. The stability order is \(\mathrm{R_2C{=}CR_2} > \mathrm{R_2C{=}CHR} > \mathrm{R_2C{=}CH_2}\), \(\mathrm{RCH{=}CHR} > \mathrm{RCH{=}CH_2}\).

  36. Substitution and elimination always compete. Tertiary halides, bulky strong bases, less polar solvents and high temperature favour elimination; primary halides, weaker bases acting as nucleophiles, polar solvents and low temperature favour substitution.

  37. Sodium, magnesium and cadmium give organometallic compounds, in which carbon is bonded directly to a metal and therefore carries a partial negative charge and behaves as a nucleophile.

  38. \(\mathrm{R\!-\!X} + \mathrm{Mg} \xrightarrow{\ \text{dry ether}\ } \mathrm{R\!-\!Mg\!-\!X}\) gives the Grignard reagent, which is destroyed by water, alcohols or ammonia and must therefore be handled under anhydrous conditions.

  39. Wurtz reaction: \(2\,\mathrm{R\!-\!X} + 2\,\mathrm{Na} \xrightarrow{\ \text{dry ether}\ } \mathrm{R\!-\!R} + 2\,\mathrm{NaX}\). Two different alkyl halides together give all three possible alkanes.

  40. Wurtz–Fittig reaction joins an aryl halide to an alkyl halide with sodium in dry ether, alkylating the ring; with only aryl halide the product is biphenyl, the Fittig reaction.

  41. Haloarenes resist nucleophilic substitution for two reasons: a lone pair of the halogen is in conjugation with the ring \(\pi\)-electrons, giving the C–X bond partial double bond character (C–Cl is 169 pm in chlorobenzene against 178 pm in an alkyl chloride), and the halogen is held by an \(\mathrm{sp^2}\) carbon. \(\mathrm{S_N}1\) is ruled out because the phenyl cation is not resonance stabilised, and \(\mathrm{S_N}2\) because the ring blocks backside attack.

  42. Chlorobenzene is converted to phenol only at about 623 K and 300 atm. Electron withdrawing groups at the ortho and/or para positions activate the halogen strongly by stabilising the negatively charged intermediate; the more such groups, the milder the conditions needed. The same group at the meta position has practically no effect.

  43. Haloarenes undergo electrophilic substitution more slowly than benzene, because the halogen deactivates the ring through its −I effect; but its +R effect raises the electron density at the ortho and para positions, so the halogen is o-/p- directing. The para product usually predominates because the ortho position is crowded.

  44. Halogenation, nitration, sulfonation and Friedel–Craft’s alkylation and acylation all follow this pattern, giving ortho and para products with para as the major one.

  45. Dichloromethane is a solvent and aerosol propellant; over exposure causes dizziness and nausea and it damages the cornea.

  46. Chloroform is used to make the refrigerant R-22, as a solvent for gums, fats and resins, and as a source of dichlorocarbene. It depresses the central nervous system, affects the liver, and forms poisonous phosgene in air and light, so it is stored in dark air-tight bottles.

  47. Carbon tetrachloride dissolves oils, fats and resins, serves as a source of chlorine and as a cleaning agent. It is highly toxic to the liver, suspected of being carcinogenic, and is a greenhouse gas.

  48. Iodoform is a yellow crystalline antiseptic used in dressings, though its use is limited; it irritates skin, eyes and the respiratory tract.

  49. Freons are chlorofluorocarbons used as refrigerants, propellants, solvents and foam blowing agents. Ultraviolet radiation splits off a chlorine atom, \(\mathrm{CFCl_3} \rightarrow \mathrm{CFCl_2} + \mathrm{Cl}\), which then destroys ozone by \(\mathrm{O_3} + \mathrm{Cl} \rightarrow \mathrm{O_2} + \mathrm{ClO}\) followed by \(\mathrm{ClO} + \mathrm{O} \rightarrow \mathrm{O_2} + \mathrm{Cl}\). Because the chlorine atom is regenerated, one atom can destroy up to 100,000 ozone molecules.

  50. DDT is a crystalline insecticide once used widely against mosquitoes and lice. It is a persistent organic pollutant: resistant to metabolism, readily absorbed through the skin, and stored in fatty tissue, so it accumulates in the ecosystem. Its use is now banned.

Flowchart

FC 10.10 – The chapter at a glance: alcohols / hydrocarbons / other halides / arenes → (preparation: HX, PX₃, PCl₅, SOCl₂; HX or X₂ addition; Finkelstein and Swartz exchange; electrophilic halogenation and Sandmeyer) → halogen derivative R–X or Ar–X → (physical properties: polar C–X bond, boiling point order RI > RBr > RCl > RF, insoluble in water) → branch A: nucleophilic substitution → S_N2 for primary halides, inversion of configuration; S_N1 for tertiary halides, racemization → alcohols, ethers, esters, amines, nitriles; branch B: elimination with alcoholic KOH → alkene, Saytzeff product major; branch C: active metals → Grignard reagent with Mg, alkane by Wurtz with Na; branch D: haloarenes → nucleophilic substitution only under forcing conditions or with o/p electron withdrawing groups, and slow electrophilic substitution giving mainly the para product; branch E: polyhalogen compounds → uses as solvents, refrigerants and insecticides, and their environmental effects.

10.9 Objective Questions

  1. The correct order of increasing reactivity of the C–X bond towards a nucleophile in the following compounds is: (I) a benzene ring bearing X; (II) a benzene ring bearing X with an \(\mathrm{{-}NO_2}\) group at the para position; (III) \(\mathrm{(CH_3)_3C\!-\!X}\); (IV) \(\mathrm{(CH_3)_2CH\!-\!X}\).
    1. I < II < III < IV
    2. II < I < III < IV
    3. III < IV < II < I
    4. IV < III < I < II
  2. The major product of the reaction \(\mathrm{CH_3\!-\!CH{=}CH_2} + \mathrm{HI} \xrightarrow{\ \text{peroxide}\ }\) is,
    1. \(\mathrm{I\!-\!CH_2\!-\!CH{=}CH_2}\)
    2. \(\mathrm{CH_3\!-\!CH_2\!-\!CH_2I}\)
    3. \(\mathrm{CH_3\!-\!CHI\!-\!CH_3}\)
    4. \(\mathrm{CH_3\!-\!CHI\!-\!CH_2OH}\)
  3. Which of the following is likely to undergo racemization during alkaline hydrolysis? (I) \(\mathrm{CH_3\!-\!CHCl\!-\!C_2H_5}\); (II) a benzene ring bearing \(\mathrm{{-}CH_2Cl}\); (III) a benzene ring bearing \(\mathrm{{-}Cl}\); (IV) \(\mathrm{CH_3\!-\!CH(CH_3)\!-\!CH_2Cl}\).
    1. Only I
    2. Only II
    3. II and IV
    4. Only IV
  4. The best method for the preparation of alkyl fluorides is
    1. Finkelstein reaction
    2. Swartz reaction
    3. Free radical fluorination
    4. Sandmeyer’s reaction
  5. Identify the chiral molecule from the following.
    1. 1-Bromobutane
    2. 1,1-Dibromobutane
    3. 2,3-Dibromobutane
    4. 2-Bromobutane
  6. An alkyl chloride on Wurtz reaction gives 2,2,5,5-tetramethylhexane. The same alkyl chloride on reduction with zinc–copper couple in alcohol gives a hydrocarbon with molecular formula \(\mathrm{C_5H_{12}}\). What is the structure of the alkyl chloride?
    1. \(\mathrm{(CH_3)_3C\!-\!CH_2Cl}\)
    2. \(\mathrm{CH_3\!-\!CCl(CH_3)\!-\!CH_2CH_3}\)
    3. \(\mathrm{CH_3\!-\!CH_2\!-\!CHCl\!-\!CH_3}\)
    4. \(\mathrm{CH_3\!-\!CH(CH_3)\!-\!CH(CH_3)\!-\!CH_2Cl}\)
  7. Butanenitrile may be prepared by heating
    1. propanol with KCN
    2. butanol with KCN
    3. n-butyl chloride with KCN
    4. n-propyl chloride with KCN
  8. Choose the compound from the following that will react fastest by \(\mathrm{S_N}1\) mechanism.
    1. 1-iodobutane
    2. 1-iodopropane
    3. 2-iodo-2-methylbutane
    4. 2-iodo-3-methylbutane
  9. For the sequence (chlorocyclohexane) \(+ \mathrm{Mg} \xrightarrow{\ \text{dry ether}\ } \mathrm{A} \xrightarrow{\ \mathrm{H_2O}\ } \mathrm{B}\), the product ‘B’ in the above reaction sequence is,
    1. cyclohexyl–Mg
    2. cyclohexyl–Mg–Cl
    3. Cl–cyclohexyl–Mg
    4. cyclohexane
  10. Which of the following is used as a source of dichlorocarbene?
  1. tetrachloromethane
  2. chloroform
  3. iodoform
  4. DDT

10.10 Check Your Concepts

  1. Classify each of the following, stating the hybridization of the carbon that carries the halogen: (i) \(\mathrm{CH_3\!-\!CH{=}CH\!-\!CH_2\!-\!Br}\), (ii) \(\mathrm{C_6H_5\!-\!CH(CH_3)\!-\!Cl}\), (iii) \(\mathrm{CH{\equiv}C\!-\!Br}\), (iv) a benzene ring bearing \(\mathrm{{-}I}\) at one position and \(\mathrm{{-}CH_3}\) at the next.

  2. Assertion–Reason. Assertion (A): Vinyl chloride does not react with aqueous \(\mathrm{KOH}\) under ordinary conditions. Reason (R): In vinyl chloride the chlorine is attached to an \(\mathrm{sp^2}\) carbon and one of its lone pairs is in conjugation with the double bond. Choose the correct option: (a) both A and R are true and R is the correct explanation of A; (b) both A and R are true but R is not the correct explanation of A; (c) A is true, R is false; (d) A is false, R is true.

  3. The \(\mathrm{C\!-\!I}\) bond enthalpy is much lower than the \(\mathrm{C\!-\!F}\) bond enthalpy. Explain the structural reason for this difference, and state one consequence it has for the reactivity of alkyl halides in nucleophilic substitution.

  4. Arrange 1-chlorobutane, 2-chlorobutane and 2-chloro-2-methylpropane in increasing order of reactivity towards the \(\mathrm{S_N}1\) mechanism, and give the reason for the order you choose.

  5. A student attempts to prepare a Grignard reagent by adding magnesium turnings to bromoethane dissolved in ethanol. Explain what will happen, write the equation for the reaction that actually takes place, and name the organic product.

  6. Predict the major product formed when 2-bromo-2-methylbutane is boiled with alcoholic \(\mathrm{KOH}\). Name the rule you have used and state why the major product is the more stable alkene.

  7. Complete the reaction and name both products, indicating which is the major one: chlorobenzene \(+\ \mathrm{Cl_2} \xrightarrow{\ \text{anhydrous}\ \mathrm{FeCl_3}\ }\). Explain why one of the two predominates.

  8. Distinguish between a geminal dihalide and a vicinal dihalide, giving one example of each, and state which of the two is obtained when an alkene reacts with bromine in \(\mathrm{CCl_4}\) at room temperature.

  9. The boiling points of the three isomeric dichlorobenzenes lie within a few kelvin of one another, but their melting points differ by nearly seventy kelvin. Explain this observation.

  10. Match the reagent in Column I with the product it gives from an alkyl halide \(\mathrm{R\!-\!X}\) in Column II.

Column I Column II
a. \(\mathrm{NaOR'}\) i. nitroalkane
b. alcoholic \(\mathrm{KCN}\) ii. primary amine
c. alcoholic \(\mathrm{AgCN}\) iii. ether
d. \(\mathrm{AgNO_2}\) iv. alkyl cyanide
e. \(\mathrm{NH_3}\) (excess, under pressure) v. isocyanide
  1. An optically active alkyl halide is hydrolysed and the product is found to have the configuration opposite to that of the starting material. Which mechanism has operated? Explain how the mechanism accounts for the change in configuration, and name the effect.

  2. Chlorobenzene needs about 623 K and 300 atm to be converted into phenol, while 2,4,6-trinitrochlorobenzene gives the corresponding phenol with merely warm water. Explain the difference.

  3. What happens when a mixture of methyl bromide and ethyl bromide is treated with sodium in dry ether? Write the products, and explain why this route is rarely used for preparing a particular alkane.

  4. A chemist needs a sample of pure 1-chlorobutane from butan-1-ol. Explain why thionyl chloride would be preferred to phosphorus pentachloride for this preparation, and write the equation for the reaction chosen.

  5. Assertion–Reason. Assertion (A): Chlorobenzene directs an incoming electrophile mainly to the para position. Reason (R): Chlorine activates the benzene ring towards electrophilic substitution. Choose the correct option: (a) both A and R are true and R is the correct explanation of A; (b) both A and R are true but R is not the correct explanation of A; (c) A is true, R is false; (d) A is false, R is true.

  6. Draw the transition state formed when methyl bromide reacts with hydroxide ion. Mark the partial bonds and the partial charges, state the number of \(\sigma\) bonds lying in one plane and the angle between them, and explain why the nucleophile must approach from the side opposite the bromine.

  7. Explain why an \(\mathrm{S_N}1\) reaction carried out on an optically active substrate gives a product that is very nearly optically inactive, while an \(\mathrm{S_N}2\) reaction on the same substrate does not.

  8. Identify A and B, and name the type of reaction in each step: propan-2-ol \(\xrightarrow{\ \text{conc. HCl, anhydrous}\ \mathrm{ZnCl_2}\ } \mathrm{A} \xrightarrow{\ \text{alcoholic KOH},\ \Delta\ } \mathrm{B}\).

  9. Which will react faster with sodium iodide in acetone — 1-chlorobutane or 2-chloro-2-methylpropane? Name the reaction, state the mechanism involved, and justify your choice.

  10. Arrange chlorobenzene, m-nitrochlorobenzene, p-nitrochlorobenzene and 2,4-dinitrochlorobenzene in increasing order of reactivity towards nucleophilic substitution, and explain why the position of the nitro group matters as much as the number of such groups.

  11. A compound with molecular formula \(\mathrm{C_4H_9Br}\) is optically active. Draw its structure, mark the chiral carbon with an asterisk and give its IUPAC name. Explain why the isomer 1-bromobutane is not optically active.

  12. Bromination of benzene with \(\mathrm{Br_2}\) and \(\mathrm{FeBr_3}\) is carried out in the dark. Explain what would happen if the reaction were exposed to bright light instead, and name the type of reaction that would then compete.

  13. Write the two equations by which a chlorine atom released from a CFC destroys ozone in the stratosphere. Explain why a single chlorine atom is able to destroy a very large number of ozone molecules, and identify the role the chlorine atom is playing.

  14. Give reasons for each of the following: (i) DDT accumulates in the fatty tissue of fish rather than being excreted; (ii) chloroform is stored in dark coloured, air-tight bottles; (iii) carbon tetrachloride, though useful as a solvent, is no longer used as a cleaning agent in schools and homes.

  15. What happens if an alkyl halide with at least one \(\beta\)-hydrogen is treated with (i) aqueous \(\mathrm{KOH}\) and (ii) alcoholic \(\mathrm{KOH}\)? Name the two competing reactions and list three factors that decide which one predominates.

  16. Write the IUPAC name of the following compounds.

  1. \(\mathrm{CH_3\!-\!CH{=}C(CH_3)\!-\!CH(CH_3)\!-\!Br}\)
  2. \(\mathrm{CH_3\!-\!CHCl\!-\!CH(CH_3)\!-\!CH_2\!-\!CH_3}\)
  3. a cyclohexane ring bearing \(\mathrm{{-}Cl}\) and \(\mathrm{{-}C_2H_5}\)
  4. a benzene ring bearing two \(\mathrm{{-}Cl}\) groups and one \(\mathrm{{-}CH_3}\) group
  1. Write the structure and IUPAC name of the major product in each of the following reactions.
  1. \(\mathrm{CH_3\!-\!CH(CH_3)\!-\!CH_2Cl} + \mathrm{NaI} \xrightarrow{\ \text{acetone}\ }\)
  2. \(\mathrm{CH_3\!-\!CH_2Br} + \mathrm{SbF_3} \rightarrow\)
  3. \(\mathrm{CH_3\!-\!CH(CH_3)\!-\!CH{=}CH_2} + \mathrm{HBr} \xrightarrow{\ \text{peroxide}\ }\)
  4. cyclohexanol \(+\ \mathrm{SOCl_2} \rightarrow\)
  5. toluene \(+\ \mathrm{Cl_2} \xrightarrow{\ \mathrm{Fe},\ \text{dark}\ }\)
  1. Identify the chiral molecule/s from the following.
  1. \(\mathrm{CH_3\!-\!CH(OH)\!-\!CH_2\!-\!CH_3}\)
  2. \(\mathrm{CH_3\!-\!CH_2\!-\!CHBr\!-\!CH_2\!-\!CH_3}\)
  3. \(\mathrm{CH_3\!-\!CH_2\!-\!CH_2\!-\!CH_2Br}\)
  4. \(\mathrm{CH_3\!-\!CH(CH_3)\!-\!CH_2\!-\!CH_3}\)
  1. Which one compound from the following pairs would undergo \(\mathrm{S_N}2\) faster?
  1. a cyclohexane ring bearing \(\mathrm{{-}CH_2Cl}\), and a cyclohexane ring bearing \(\mathrm{{-}Cl}\)
  2. \(\mathrm{CH_3CH_2CH_2I}\) and \(\mathrm{CH_3CH_2CH_2Cl}\)
  1. Complete the following reactions giving the major product.
  1. \(\mathrm{CH_3\!-\!CH{=}CH_2} \xrightarrow{\ \mathrm{HBr},\ \text{peroxide}\ } \mathrm{A} \xrightarrow{\ \text{alc. KOH}\ } \mathrm{B}\)
  2. \(\mathrm{CH_3\!-\!CH(OH)\!-\!CH_3} \xrightarrow{\ \text{Red P}/\mathrm{Br_2}\ } \mathrm{A} \xrightarrow{\ \mathrm{Ag_2O}/\mathrm{H_2O}\ } \mathrm{B}\)
  3. \(\mathrm{(CH_3)_3C\!-\!CH_2\!-\!Cl} \xrightarrow{\ \mathrm{Na}/\text{dry ether}\ } \mathrm{A}\)
  4. (chlorobenzene) \(\xrightarrow{\ \mathrm{Mg}/\text{dry ether}\ } \mathrm{A}\)
  1. Name the reagent used to bring about the following conversions.
  1. Bromoethane to ethoxyethane
  2. 1-Chloropropane to 1-nitropropane
  3. Ethyl bromide to ethyl isocyanide
  4. Chlorobenzene to biphenyl
  1. Arrange the following in the increasing order of boiling points.
  1. 1-Bromopropane
  2. 2-Bromopropane
  3. 1-Bromobutane
  4. 1-Bromo-2-methylpropane
  1. Match the pairs.
Column I Column II
a. \(\mathrm{CH_3\!-\!CHX\!-\!CH_3}\) i. vinyl halide
b. \(\mathrm{CH_2{=}CH\!-\!CH_2X}\) ii. alkyl halide
c. \(\mathrm{CH_2{=}CH\!-\!X}\) iii. allyl halide
iv. benzyl halide
v. aryl halide
  1. Give reasons.
  1. Haloarenes are less reactive than haloalkanes.
  2. Alkyl halides, though polar, are immiscible with water.
  3. Reactions involving Grignard reagent must be carried out under anhydrous conditions.
  4. Alkyl halides are generally not prepared by free radical halogenation of alkanes.
  1. Distinguish between \(\mathrm{S_N}1\) and \(\mathrm{S_N}2\) mechanisms of substitution reaction.

  2. Explain optical isomerism in 2-chlorobutane.

  3. Convert the following.

  1. Propene to propan-1-ol
  2. Benzyl alcohol to benzyl cyanide
  3. Ethanol to propane nitrile
  4. But-1-ene to n-butyl iodide
  5. 2-Chloropropane to propan-1-ol
  6. tert-Butyl bromide to isobutyl bromide
  7. p-Nitrochlorobenzene to p-nitrophenol
  8. Propene to 1-nitropropane
  1. HCl is added to a hydrocarbon ‘A’ \((\mathrm{C_4H_8})\) to give a compound ‘B’, which on hydrolysis with aqueous alkali forms the tertiary alcohol ‘C’ \((\mathrm{C_4H_{10}O})\). Identify ‘A’, ‘B’ and ‘C’.

  2. Complete the following reaction sequences by writing the structural formulae of the organic compounds ‘A’, ‘B’ and ‘C’.

  1. 2-Bromobutane \(\xrightarrow{\ \text{alc. KOH}\ } \mathrm{A} \xrightarrow{\ \mathrm{Br_2}\ } \mathrm{B} \xrightarrow{\ \mathrm{NaNH_2}\ } \mathrm{C}\)
  2. Isopropyl alcohol \(\xrightarrow{\ \mathrm{PBr_3},\ \Delta\ } \mathrm{A} \xrightarrow{\ \mathrm{NH_3}\ \text{excess}\ } \mathrm{B}\)
  1. Observe the following and answer the questions given below. \[\mathrm{CH_2{=}CH\!-\!\ddot{X}\!:} \longleftrightarrow {}^{\ominus}\mathrm{CH_2\!-\!CH{=}\overset{\oplus}{X}\!:}\]
  1. Name the type of halogen derivative.
  2. Comment on the bond length of the C–X bond in it.
  3. Can it react by \(\mathrm{S_N}1\) mechanism? Justify your answer.