Whiteboard Chemistry with Joe White

Carboxylic Acids & Derivatives

Carboxylic acids as weak acids, esters and esterification, the two hydrolysis routes with fats, soap and biodiesel, and the acylating agents — acyl chlorides and acid anhydrides — through the nucleophilic addition–elimination mechanism.

AQA 7404/7405 Paper 2 A-level only
R C O Cl OH OR NH₂
Where this sits

Oxidising an aldehyde (from 3.3.8) gives a carboxylic acid, and this page follows the family that grows from it. The unifying idea is the acyl group, R–C(=O)–: swap what is attached to it and you move between the acid, ester, acyl chloride, acid anhydride and amide. One mechanism — nucleophilic addition–elimination — links most of them.

Carboxylic acids

Carboxylic acids contain the –COOH group. The C=O and O–H make the group strongly polar, so carboxylic acids hydrogen-bond — to each other (high boiling points) and to water (the short-chain acids are very soluble).

They are weak acids — only partially dissociated in water — but they are acidic enough to show the usual reactions:

  • with carbonates and hydrogencarbonates they release CO2 (effervescence) — the test that distinguishes a carboxylic acid from a phenol or an alcohol;
  • with metals and bases they form carboxylate salts.
H₃C C O O H the acidic H in water H₃C C O O + H + weak acid — the equilibrium lies well to the left
Only a carboxylic acid (not a phenol or alcohol) fizzes with a carbonate.
Exam questions

Compounds V, W, X and Y are isomers with the molecular formula C5H10O2. Isomers V and W are carboxylic acids with formulas that can be written as C4H9COOH.

Q1a [1 mark]

Give an equation for the reaction of C4H9COOH with sodium hydrogencarbonate.

Show answer

C4H9COOH + NaHCO3 → C4H9COONa + CO2 + H2O 1 mark

Q1b [1 mark]

Isomer V has an asymmetric carbon atom. Deduce the structure of V.

Show answer

CH3CH2CH(CH3)COOH 1 mark

2-methylbutanoic acid — the CH carbon carries four different groups (CH3, C2H5, COOH and H), so it is the asymmetric centre. Later parts of this question deduce the other isomers from their 1H NMR spectra — that skill lives in NMR (3.3.15).

Source: AQA A-Level Chemistry past papers.

Esters & esterification

Esters have the group –COO– and are named alkyl alkanoate — the alkyl part comes from the alcohol, the alkanoate part from the acid. So ethanoic acid + ethanol gives ethyl ethanoate.

Naming, in two halves

Ethyl ethanoate, CH3COOC2H5: ethyl = the C2H5 from ethanol; ethanoate = the CH3COO from ethanoic acid. Write the alcohol-derived group first, the acid-derived group second.

Warmed with an alcohol and a concentrated sulfuric acid catalyst, a carboxylic acid forms an ester. The reaction — esterification — is reversible, so the mixture reaches an equilibrium and the yield is never complete:

H₃C C O O H + C₂H₅ O H lost as part of the water lost as H conc H₂SO₄ (catalyst) H₃C C O O C₂H₅ + H₂O the ester link, –COO–
The water forms from the acid’s –OH and the alcohol’s H; the rest joins as the ester link.

Making an ester in the lab

The ester preparation is a favourite practical question, and every step has a purpose you must be able to state — vague answers about “purifying” do not score:

Preparing ethyl ethanoate — each step and why it is done
StepWhy it is done
Reflux the acid + alcohol + conc H2SO4 (anti-bumping granules)The catalyst speeds the reaction; reflux heats the flammable mixture without losing vapour — heat with a water bath or electric heater, never a flame.
Distil off the productThe ester has the lowest boiling point (no hydrogen bonding between ester molecules) — collect the fraction over the ester’s boiling range.
Shake with aqueous sodium carbonate in a separating funnelNeutralises / removes the acid impurities; the CO2 produced builds pressure, so release the pressure regularly.
Separate the layersThe ester is immiscible with water and less dense, so it forms the upper layer; run off and discard the aqueous layer.
Add anhydrous CaCl2 or MgSO4A drying agent — removes water. (Say “drying agent / removes water”, never “dehydrates”.)
Redistil, collecting over a narrow rangeA sharp boiling point matching the data-book value confirms purity.
Worked example — limiting reagent and percentage yield

14.8 g of butan-1-ol (Mr = 74.0) is warmed with 15.0 g of ethanoic acid (Mr = 60.0) and a concentrated sulfuric acid catalyst; 8.7 g of butyl ethanoate (Mr = 116.0) is collected. Find the percentage yield.

Step 1 — moles of each reactant:

n(butan-1-ol) = 14.8 ÷ 74.0 = 0.200 mol n(ethanoic acid) = 15.0 ÷ 60.0 = 0.250 mol

Step 2 — identify the limiting reagent. The equation is 1 : 1, so butan-1-ol (0.200 mol) runs out first — it is limiting.

Step 3 — theoretical mass of ester from the limiting reagent:

0.200 × 116.0 = 23.2 g

Step 4 — percentage yield:

(8.7 ÷ 23.2) × 100 = 37.5 %

Yields are low because esterification is an equilibrium — and more is lost in the separating funnel and distillations.

Uses of esters

Their pleasant smells and low reactivity make esters useful as solvents, plasticisers, and in perfumes and food flavourings.

Exam questions

Ethyl ethanoate can be made by reacting ethanol with ethanoic acid in the presence of concentrated sulfuric acid.

Method

  1. A mixture of ethanol, ethanoic acid, and concentrated sulfuric acid, with anti-bumping granules, is heated under reflux for 10 minutes.
  2. The apparatus is rearranged for distillation.
  3. The mixture is heated to collect the liquid that distils between 70 and 85 °C
  4. The distillate is placed in a separating funnel. Aqueous sodium carbonate is added, and a stopper is placed in the funnel. The mixture is shaken, releasing pressure as necessary.
  5. The lower aqueous layer is removed and the upper organic layer is placed in a small conical flask.
  6. Anhydrous calcium chloride is added to the sample in the conical flask. The flask is shaken well and left for a few minutes.
  7. The liquid from the flask is redistilled and the distillate is collected between 74 and 79 °C
Q2a [1 mark]

State the role of concentrated sulfuric acid in this reaction.

Show answer

Catalyst. 1 mark

Allow “reduces Ea”. Ignore “speeds up reaction”, “provides alternative path”, “proton donor” and “dehydrating agent” on their own.

Q2b [1 mark]

The reaction mixture is flammable. Suggest how the reaction mixture should be heated in step 1.

Show answer

Electric heater / heating mantle or (hot) water bath. 1 mark

“Not with a Bunsen / naked flame” on its own is ignored — you must say what is used. Any indication of direct heat from a Bunsen loses the mark.

Q2c [2 marks]

State why sodium carbonate is added to the distillate in step 4. Explain why there is a build-up of pressure in the separating funnel.

Show answer

M1 — to neutralise / react with / remove the acid. 1 mark

M2 — carbon dioxide / gas is produced. 1 mark

Either acid (ethanoic and/or sulfuric) is allowed for M1; naming the wrong acid or the wrong gas scores nothing. “Effervescence / bubbles” is allowed for M2.

Q2d [2 marks]

Give a reason why two layers form in the separating funnel. Suggest why ethyl ethanoate forms the upper layer.

Show answer

M1 — ethyl ethanoate is immiscible with / insoluble in water. 1 mark

M2 — ethyl ethanoate is less dense / has a lower density (than water). 1 mark

“Lighter” is not accepted for M2, and “different / low density” is ignored — compare it to water.

Q2e [1 mark]

State why anhydrous calcium chloride is added in step 6.

Show answer

To remove / absorb water — a drying agent. 1 mark

“Dehydrates” is ignored, and “to dry the reactants” or “to remove soluble impurities” is not accepted — it dries the product.

Q2f [5 marks]

A student uses the method to prepare some ethyl ethanoate. The student adds 10.0 cm3 of ethanol (Mr = 46.0) to 5.25 g of ethanoic acid (Mr = 60.0) and obtains 5.47 g of ethyl ethanoate (Mr = 88.0). For ethanol, density = 0.790 g cm−3. Determine the limiting reagent. Calculate the percentage yield of ethyl ethanoate.

Show answer

M1 — mass of ethanol = 10 × 0.790 (= 7.90 g) 1 mark

M2 — n(ethanol) = 7.90 ÷ 46.0 (= 0.172 mol) and n(ethanoic acid) = 5.25 ÷ 60.0 (= 0.0875 mol) 1 mark

M3 — (limiting reagent is) ethanoic acid. 1 mark

M4 — max mass of ethyl ethanoate = 88.0 × 0.0875 (= 7.70 g) 1 mark

M5 — % yield = (5.47 ÷ 7.70) × 100 = 71.0 % 1 mark

70.6 to 71.1 (to a minimum of 2 s.f.) is accepted, with error carried forward at each stage. M2 needs the numbers or sums for both substances; M4 is independent of M3.

Q2g [1 mark]

Suggest a reason why the percentage yield is not 100%.

Show answer

The reaction is an equilibrium / reversible. 1 mark

Losses during distillation / isolation / transfer, incomplete reaction, or side reactions are also allowed. “Water is also produced” is ignored.

The original question also asks you to spot two mistakes in a printed diagram of the reflux set-up (bung in the condenser; water connected the wrong way) — reflux apparatus is drawn on the required practicals page.

Q3 [2 marks]

Ester F can be prepared from propan-2-ol and ethanoic acid. Give an equation for this reaction. Name ester F.

Show answer

M1 — CH3CH(OH)CH3 + CH3COOH ⇌ CH3COOCH(CH3)2 + H2O 1 mark

M2 — propan-2-yl ethanoate. 1 mark

Other valid names are allowed: 1-methylethyl ethanoate, isopropyl ethanoate, 2-propyl ethanoate. The ethanoate half must come from the acid.

Source: AQA A-Level Chemistry past papers.

Hydrolysis, fats & soap

Hydrolysis splits an ester back apart. Which products you get depends on the conditions:

  • Acid hydrolysis (dilute acid, heat under reflux) is the reverse of esterification, so it is reversible and reaches an equilibrium — giving the carboxylic acid + alcohol.
  • Alkaline hydrolysis (aqueous NaOH, heat under reflux) goes to completion, because the carboxylate salt formed does not react back — giving the carboxylate salt + alcohol.

Fats, oils, soap & biodiesel

Vegetable oils and animal fats are triesters (triglycerides) of propane-1,2,3-triol (glycerol) with three long-chain carboxylic (fatty) acids. Their ester chemistry is the ester chemistry above, three times over:

  • Alkaline hydrolysis of a fat or oil gives soap — the sodium or potassium salts of the long-chain carboxylic acids — plus glycerol. (This is saponification, the reaction soap-making has used for millennia.)
  • Biodiesel is a mixture of methyl esters of long-chain carboxylic acids, made by reacting vegetable oils with methanol in the presence of a catalyst — the methanol displaces the glycerol from the ester links (a transesterification).
Worked example — the two triglyceride equations

Write the equations for making soap and biodiesel from a triglyceride whose three R groups are identical.

Step 1 — soap (alkaline hydrolysis). Three NaOH cut the three ester links; the salt is the soap:

(RCOO)3C3H5 + 3NaOH → 3RCOONa+ + CH2(OH)CH(OH)CH2OH

Step 2 — biodiesel (transesterification). Three methanol swap in; no water is involved:

(RCOO)3C3H5 + 3CH3OH → 3RCOOCH3 + CH2(OH)CH(OH)CH2OH

Both release glycerol — count your products: three salt/ester molecules per triglyceride, one glycerol.

RCOO CH₂ RCOO CH RCOO CH₂ three ester links — a triester of glycerol + 3NaOH heat 3 RCOO⁻Na⁺ soap — salts of the long-chain acids + CH₂ OH CH OH CH₂ OH glycerol (propane-1,2,3-triol)
Saponification goes to completion because the carboxylate salt cannot re-esterify.
Exam questions

Coconut oil contains a triester with three identical R groups. This triester reacts with potassium hydroxide.

RCOO CH₂ RCOO CH RCOO CH₂ + 3KOH 3RCOOK +
Q4a [3 marks]

Complete the equation by drawing the structure of the other product of this reaction in the box. Name the type of compound shown by the formula RCOOK. Give one use for this type of compound.

Show answer

CH2OHCH(OH)CH2OH 1 mark

(Potassium) carboxylate salt. 1 mark

Soap. 1 mark

“Fatty acid salt” / “salt of a carboxylic acid” is allowed for the type; “detergent / surfactant” is allowed for the use.

Q4b [3 marks]

The triester in coconut oil has a relative molecular mass, Mr = 638.0. In the equation shown at the start of this question, R represents an alkyl group that can be written as CH3(CH2)n. Deduce the value of n in CH3(CH2)n. Show your working.

Show answer

M1 — 638 = 173 + 3(15 + 14n) — the Mr of the ester fragment (the backbone plus three COO groups) is 173 1 mark

M2 — 638 − 173 − 3(15) = 420, then divide by 3 × 14 = 42 1 mark

M3 — n = 10 (n must be an integer). 1 mark

Q4c [6 marks]

A 1.450 g sample of coconut oil is heated with 0.421 g of KOH in aqueous ethanol until all of the triester is hydrolysed. The mixture is cooled. The remaining KOH is neutralised by exactly 15.65 cm3 of 0.100 mol dm−3 HCl. Calculate the percentage by mass of the triester (Mr = 638.0) in the coconut oil.

Show answer

M1 — n(HCl) = 0.100 × 0.01565 = 1.565 × 10−3 mol 1 mark

M2 — initial n(KOH) = 0.421 ÷ 56.1 = 7.50 × 10−3 mol 1 mark

M3 — n(KOH) used = M2 − M1 = 5.939 × 10−3 mol 1 mark

M4 — n(ester) = M3 ÷ 3 = 1.980 × 10−3 mol 1 mark

M5 — mass of ester = 1.980 × 10−3 × 638 = 1.263 g 1 mark

M6 — % by mass = (1.263 ÷ 1.450) × 100 = 87.1 % 1 mark

87.0 to 87.1 is allowed (2 s.f. accepted); an answer above 100% cannot score M6. This is a back titration — the HCl counts the KOH left over, and each triester molecule used three KOH.

Q4d [3 marks]

Suggest why aqueous ethanol is a suitable solvent when heating the coconut oil with KOH. Give a safety precaution used when heating the mixture. Justify your choice.

Show answer

M1 — it dissolves both the oil and the KOH — a mutual solvent, so the reactants are miscible. 1 mark

M2 — use a water bath (or electric heater / mantle / sand bath) for heating. 1 mark

M3 — ethanol is flammable — this prevents the risk of fire. 1 mark

The precaution must be linked to heating, and the justification must match the precaution given.

The diagram below shows an incomplete mechanism for the reaction of an ester with aqueous sodium hydroxide.

H₃C C O O CH₃ OH H₃C C O O CH₃ OH H₃C C O O H H₃C O H₃C C O O + CH₃OH step 1 step 2 step 3
Q5a [3 marks]

Add three curly arrows to complete the mechanism in the diagram.

Show answer

M1 — arrow from the C=O bond to the O. 1 mark

M2 — arrow from the correct C–O bond to the O. 1 mark

M3 — arrow from the O–H bond to the O. 1 mark

H₃C C O O CH₃ OH H₃C C O O CH₃ OH H₃C C O O H H₃C O M1 M2 M3

You are not expected to recall this mechanism — the question supplies it, and the skill is placing arrows precisely: each starts at a bond midpoint and lands on the oxygen gaining the electrons.

Q5b [1 mark]

Name the type of reaction shown in the diagram.

Show answer

(Alkaline / base) hydrolysis. 1 mark

Q5c [1 mark]

Deduce the role of the CH3O ion in step 3 shown in the diagram.

Show answer

Base. 1 mark

“Proton acceptor” is allowed — in step 3 it takes the H+ from the carboxylic acid.

Q5d [1 mark]

A triester in vegetable oil reacts with sodium hydroxide in a similar way. Give a use for a product of this reaction.

Show answer

Soap. 1 mark

“Soap only” — the mark scheme accepts nothing else here.

Source: AQA A-Level Chemistry past papers.

Acyl chlorides & acid anhydrides

Replace the –OH of a carboxylic acid with –Cl and you get an acyl chloride (e.g. ethanoyl chloride, CH3COCl); join two acid molecules with loss of water and you get an acid anhydride (e.g. ethanoic anhydride, (CH3CO)2O). Both are acylating agents: they hand the acyl group CH3CO– to a nucleophile, far faster than the acid itself would. Acyl chlorides are the more reactive of the two. The third derivative to recognise is the amide, RCONH2 — the nitrogen-containing product below.

The four nucleophiles — one pattern

Each of the four common nucleophiles attacks the acyl group and displaces the leaving group. The product is set by the nucleophile:

Reactions of ethanoyl chloride, CH3COCl, with the four nucleophiles
NucleophileOrganic productEquation
Watercarboxylic acidCH3COCl + H2O → CH3COOH + HCl
Alcohol (e.g. ethanol)esterCH3COCl + C2H5OH → CH3COOC2H5 + HCl
AmmoniaamideCH3COCl + 2NH3 → CH3CONH2 + NH4Cl
Primary amine (e.g. CH3NH2)N-substituted amideCH3COCl + 2CH3NH2 → CH3CONHCH3 + CH3NH3Cl
Aromatic amine — phenylamine, C6H5NH2N-phenyl-substituted amideCH3COCl + 2C6H5NH2 → CH3CONHC6H5 + C6H5NH3Cl

An acid anhydride does the same four reactions, just more gently — its leaving group is the ethanoate ion, so the by-product is ethanoic acid instead of HCl.

Precision points — ammonia and amines need two equivalents

One molecule of the nucleophile forms the product; a second mops up the HCl released (as NH4+Cl or the alkylammonium salt). Balance the equation with 2NH3 / 2 amine, not one.

The mechanism: nucleophilic addition–elimination

Every one of those reactions goes by the same two-stage mechanism. The carbonyl carbon is Cδ+ (electron-poor), so:

  1. Addition: the nucleophile’s lone pair attacks Cδ+; the C=O π bond breaks onto the oxygen, giving a tetrahedral intermediate with the negative charge on that oxygen.
  2. Elimination: the C=O reforms and pushes out the leaving group (Cl from an acyl chloride, or the carboxylate from an anhydride); the nucleophile then loses H+ to give the neutral product.
STEP 1 addition H₃C C O Cl O H H δ+ δ− δ− STEP 2 elimination H₃C C O Cl O H H + STEP 3 products H₃C C O OH + HCl ethanoic acid misty fumes
The name to write is nucleophilic addition–elimination — not substitution.
Worked example — acylation of an amine

Ethanoyl chloride reacts with methylamine. Name the mechanism and the organic product, and write the balanced equation.

Step 1 — the mechanism is nucleophilic addition–elimination (the amine’s nitrogen lone pair attacks Cδ+).

Step 2 — build the product. The nucleophile replaces the Cl: CH3CO– joins –NHCH3, giving CH3CONHCH3 — an amide with a methyl on the nitrogen, so it is named N-methylethanamide.

Step 3 — balance with the second equivalent of amine mopping up the HCl:

CH3COCl + 2CH3NH2 → CH3CONHCH3 + CH3NH3Cl

Observations — how acyl chlorides give themselves away

Acyl chlorides react violently with cold water, giving off misty fumes of HCl. Add aqueous silver nitrate and the chloride released gives an immediate white precipitate of AgCl — a chloroalkane, by contrast, barely reacts at room temperature. Acid anhydrides react with water too, but slowly and controllably, and produce no HCl.

Aspirin & Required Practical 10

Aspirin is made by acylating salicylic acid (2-hydroxybenzenecarboxylic acid) — its phenol –OH is the nucleophile, and industry uses ethanoic anhydride as the acylating agent:

Why the anhydride is preferred for aspirin

Ethanoic anhydride is less corrosive than ethanoyl chloride, is less vulnerable to hydrolysis, and does not form HCl — the only by-product is (weak) ethanoic acid.

Those three are the creditworthy reasons. AQA mark schemes have explicitly ignored answers about cost, safety in general, volatility or “less violent” — give a specific chemical advantage, not a vague one.

Required practical 10 — preparation of a pure organic solid and liquid

The solid half is aspirin: made by the acylation above, then purified by recrystallisation:

  • Dissolve the impure solid in the minimum volume of hot solvent — the minimum volume means the solution is saturated, so crystals form when it cools. Heat on a water bath.
  • Filter hot (through a warmed funnel) — removes the insoluble impurities; hot, so the product stays dissolved instead of crystallising in the funnel.
  • Cool the filtrate in an ice bath — the pure product crystallises out of the saturated solution.
  • Filter under reduced pressure (Büchner funnel and side-arm flask) — fast, and pulls the impure solution away from the crystals.
  • Wash the crystals with a little cold solvent, then leave them to dry.
  • Check purity by melting point: pure aspirin melts sharply at the data-book value; an impure sample melts lower and over a range.
Where each kind of impurity leaves
ImpurityRemoved atHow
Insolublethe hot filtrationnever dissolved — trapped on the filter paper while the product passes through in solution
Solublethe cold filtration + cold washstay dissolved in the filtrate — there is too little of them ever to saturate the cooled solution, so they never crystallise

The liquid half of the practical is the ester preparation in the esters section. Full method notes on the required practicals page.

1 · impure solid

The product plus both kinds of impurity — insoluble (filled) and soluble (rings).

2 · dissolve · minimum hot solvent

Hot, so everything soluble dissolves; minimum volume, so the solution is saturated — that is what makes crystals form on cooling. Heat on a water bath.

3 · filter hot

Insoluble impurities removed — they never dissolved, so they are trapped on the paper. Filter hot so no product crystallises in the funnel.

4 · cool in an ice bath

The product crystallises out of the saturated solution. The soluble impurities stay dissolved — too little of them ever to saturate the solution.

5 · filter under reduced pressure

to pump

Soluble impurities removed — they leave in the filtrate. Wash the crystals with a little cold solvent: cold, so the product does not redissolve.

6 · dry

Leave to dry, then check the melting point: sharp and at the data-book value = pure.

Recrystallisation, step by step — ink = the product; filled lumps = insoluble impurities (leave at step 3); open rings = soluble impurities (leave at step 5).
Exam questions
Q6 [2 marks]

Silver nitrate solution can be used to distinguish between propanoyl chloride and 1-chloropropane. Give the observations you would expect when a few drops of silver nitrate solution are added to separate samples of propanoyl chloride and 1-chloropropane.

Show answer

M1 — propanoyl chloride: misty / white / steamy fumes or an (immediate) white precipitate forms. 1 mark

M2 — 1-chloropropane: no visible change (or a white precipitate forms only slowly). 1 mark

The contrast is the point: the C–Cl bond in the acyl chloride is attacked at once by the water in the reagent, releasing Cl; the chloroalkane needs prolonged warming.

Q7 [1 mark]

Which compound reacts with warm dilute aqueous sodium hydroxide?

  1. C6H6
  2. CH3CH=CH2
  3. CH3CH2CH2NH2
  4. (CH3CO)2O

Aspirin can be produced by reacting salicylic acid with ethanoic anhydride. An incomplete method to determine the yield of aspirin is shown.

  1. Add about 6 g of salicylic acid to a weighing boat.
  2. Place the weighing boat on a 2 decimal place balance and record the mass.
  3. Tip the salicylic acid into a 100 cm3 conical flask.
  4. ______________________________________________
  5. Add 10 cm3 of ethanoic anhydride to the conical flask and swirl.
  6. Add 5 drops of concentrated phosphoric acid.
  7. Warm the flask for 20 minutes.
  8. Add ice-cold water to the reaction mixture and place the flask in an ice bath.
  9. Filter off the crude aspirin from the mixture and leave it to dry.
  10. Weigh the crude aspirin and calculate the yield.
Q8a [2 marks]

Describe the instruction that is missing from step 4 of the method. Justify why this step is necessary.

Show answer

M1 — (re)weigh the empty boat. 1 mark

M2 — in order to calculate the (exact) mass of salicylic acid added to the reaction mixture. 1 mark

Q8b [1 mark]

Suggest a suitable piece of apparatus to measure out the ethanoic anhydride in step 5.

Show answer

A 10 cm3 measuring cylinder, or a 10 cm3 pipette, burette / graduated pipette, or a 10 cm3 syringe. 1 mark

Q8c [1 mark]

Identify a hazard of using concentrated phosphoric acid in step 6.

Show answer

Corrosive. 1 mark

“Skin burn / permanent eye damage” is allowed; “irritant” and “toxic” are ignored.

Q8d [1 mark]

Complete the equation for the reaction of salicylic acid with ethanoic anhydride to produce aspirin.

COOH OH salicylic acid + COOH O C O CH₃ aspirin +
Show answer

Left-hand side: + (CH3CO)2O Right-hand side: + CH3COOH 1 mark

Q8e [5 marks]

A 6.01 g sample of salicylic acid (Mr = 138.0) is reacted with 10.5 cm3 of ethanoic anhydride (Mr = 102.0). In the reaction the yield of aspirin is 84.1%. The density of ethanoic anhydride is 1.08 g cm−3. Show by calculation which reagent is in excess. Calculate the mass, in g, of aspirin (Mr = 180.0) produced.

Show answer

M1 — n(salicylic acid) = 6.01 ÷ 138 = 4.36 × 10−2 mol 1 mark

M2 — mass of (CH3CO)2O = 10.5 × 1.08 = 11.34 g 1 mark

M3 — n((CH3CO)2O) = 11.34 ÷ 102 = 1.11 × 10−1 mol 1 mark

M4 — (CH3CO)2O is in excess. 1 mark

M5 — mass of aspirin = 4.36 × 10−2 × 0.841 × 180 = 6.59 g 1 mark

You must show and state that the ethanoic anhydride is in excess; 2 s.f. or more is allowed for the final mass.

Q8f [2 marks]

Suggest two ways in which the melting point of the crude aspirin collected in step 9 would differ from the melting point of pure aspirin.

Show answer

M1 — the value is lower. 1 mark

M2 — it melts over a range of values / the melting point is not sharp. 1 mark

Q8g [2 marks]

The crude aspirin can be purified by recrystallisation using hot ethanol (boiling point = 78 °C) as the solvent. Describe two important precautions when heating the mixture of ethanol and crude aspirin.

Show answer

M1 — (ethanol is flammable so) use a water bath to heat / do not use a Bunsen burner. 1 mark

M2 — heat to a temperature below the boiling point (so the ethanol does not boil away) / use the minimum volume of solvent. 1 mark

M1 must give the practical step — just stating the hazard scores nothing.

Q8h [1 mark]

The pure aspirin is filtered under reduced pressure. A small amount of cold ethanol is then poured through the Buchner funnel. Explain the purpose of adding a small amount of cold ethanol.

Show answer

To remove any soluble impurities (washing them away) — the ethanol is cold and little is used so that the aspirin itself does not dissolve. 1 mark

Q8i [1 mark]

A sample of the crude aspirin is kept to compare with the purified aspirin. Describe one difference in appearance you would expect to see between these two solid samples.

Show answer

The pure product will have (larger) crystals / needle-like crystals / be lighter in colour. 1 mark

Whiter, less grey, more crystalline, less powdery or shinier are all allowed — but the difference must be tied to the pure (or crude) product.

Aspirin is produced from 2-hydroxybenzenecarboxylic acid by reaction with ethanoic anhydride in the presence of concentrated phosphoric acid. The flask is heated to 85 °C for 10 minutes.

Q9a [1 mark]

Aspirin can also be produced by reacting 2-hydroxybenzenecarboxylic acid with ethanoyl chloride. State why ethanoic anhydride is preferred to ethanoyl chloride for this preparation.

Show answer

Ethanoic anhydride is less / not corrosive; or it does not form a strong acid / HCl (it only forms weak ethanoic acid); or it is less / not vulnerable to hydrolysis. 1 mark

The reverse argument about ethanoyl chloride is allowed. Cost, volatility, “safer / less toxic” and “less exothermic / violent / vigorous” are all ignored.

Q9b [1 mark]

Give the name of the mechanism for the reaction of 2-hydroxybenzenecarboxylic acid with ethanoic anhydride.

Show answer

(Nucleophilic) addition–elimination. 1 mark

“Esterification” and “acylation” are ignored — the question asks for the mechanism.

Q9c [1 mark]

Suggest the role of the concentrated phosphoric acid.

Show answer

Catalyst. 1 mark

“Speeds up the reaction / lowers activation energy” is allowed; “proton donor” is ignored.

Q9d [1 mark]

Suggest why reflux is not essential when the flask is heated to 85 °C for 10 minutes.

Show answer

The boiling points (of the reactants and products) are above 85 °C — nothing would boil / no volatile reagents. 1 mark

Source: AQA A-Level Chemistry past papers.

The derivatives map

Pull the whole topic together around the acyl group. Reactivity runs acyl chloride > acid anhydride > ester > carboxylic acid/amide — the better the leaving group, the more reactive the acylating agent. Reading the map is the exam skill: name the reagent that makes each product, and vice versa.

acyl chloride acid anhydride the acylating agents ethanoic acid ethyl ethanoate ethanamide N-methylethanamide CH₃COCl (CH₃CO)₂O CH₃COOH · carboxylic acid CH₃COOC₂H₅ · ester CH₃CONH₂ · amide CH₃CONHCH₃ · N-sub amide by-product: HCl corrosive, misty fumes by-product: ethanoic acid no corrosive fumes + H₂O + C₂H₅OH + 2NH₃ + 2CH₃NH₂ reactivity: acyl chloride > acid anhydride > ester > acid / amide
The whole topic on one map: pick the nucleophile, read off the product. With the acyl chloride the by-product is corrosive HCl; the anhydride gives ethanoic acid instead.
Precision points
  • Name the mechanism nucleophilic addition–elimination — not substitution, not “esterification” (mark schemes ignore both when the mechanism is asked for).
  • Examiner reports note that “hydrolysis” itself is poorly known — be able to define it (splitting with water) and to give the different products of the acid route (acid + alcohol, reversible) and the alkaline route (carboxylate salt + alcohol, one-way).
  • In purification steps, say what each stage removes and how — washing (removes soluble impurities) is not drying (removes water), and a drying agent never “dehydrates”.
  • Purity of aspirin is checked by melting point, never boiling point: pure = sharp and matches the data-book value; impure = lower and over a range.
  • Remember the second equivalent of NH3 / amine that removes the HCl — the equation must balance.
  • For an acyl chloride and water: violent reaction, misty HCl fumes, and an immediate white precipitate with AgNO3.
Which reagent makes which — reactions of ethanoyl chloride / ethanoic anhydride
Add this nucleophileGet this productProduct type
WaterCH3COOHcarboxylic acid
AlcoholCH3COORester
AmmoniaCH3CONH2amide
Primary amineCH3CONHRN-substituted amide

Capstone quiz — six past-paper questions

Six real AQA multiple-choice questions on this topic, in the style that opens Paper 3. Pick one answer each — the reasoning appears once you commit.

Q1 [1 mark]

Which statement about (CH3)2CHCH2COOH is correct?

  1. In aqueous solution it reacts with magnesium to form carbon dioxide.
  2. It can form hydrogen bonds.
  3. It has optical isomers.
  4. It has the IUPAC name 2-methylbutanoic acid.
Q2 [1 mark]

Which compound is formed when phenyl benzenecarboxylate is hydrolysed under acidic conditions?

  1. C6H5CH2OH
  2. C6H5CHO
  3. C6H5COCH3
  4. C6H5COOH
Q3 [1 mark]

Which compound is an amide?

  1. CH3CH2CH2CN
  2. CH3CONHCH2CH3
  3. CH3COOCH2CH3
  4. CH3NHCH2CH2CH3
Q4 [1 mark]

Compound Y has the structural formula CH3COOCH2CH(CH3)2. Which compound is a position isomer of Y?

  1. 5-hydroxyhexan-3-one
  2. butyl ethanoate
  3. hexanoic acid
  4. propyl propanoate
Q5 [1 mark]

Which reaction involves addition–elimination?

  1. (CH3)2CHBr + KOH → CH3CH=CH2 + KBr + H2O
  2. CH3COCl + C6H5OH → CH3COOC6H5 + HCl
  3. CH3CH=CH2 + Cl2 → CH3CHClCH2Cl
  4. CH3CH2CH2Br + NaOH → CH3CH2CH2OH + NaBr
Q6 [1 mark]

Which compound forms a white precipitate when added to aqueous silver nitrate?

  1. bromoethane
  2. ethanal
  3. ethanoic anhydride
  4. ethanoyl chloride

Source: AQA A-Level Chemistry past papers.

3.3.9 Carboxylic acids & derivatives — Quick-reference summary
  • Carboxylic acids (–COOH) are weak acids: they liberate CO2 from carbonates (the distinguishing test) and form carboxylate salts with metals and bases; they hydrogen-bond, so the short-chain acids are soluble.
  • Esterification: carboxylic acid + alcohol ⇌ ester + water (conc H2SO4 catalyst, reversible). Esters are named alkyl alkanoate; used as solvents, plasticisers, perfumes and food flavourings.
  • Ester hydrolysis: acid hydrolysis is reversible (→ acid + alcohol); alkaline hydrolysis goes to completion (→ carboxylate salt + alcohol).
  • Fats and oils are triesters of glycerol (propane-1,2,3-triol). Alkaline hydrolysis gives soap (salts of long-chain carboxylic acids) + glycerol; biodiesel is the methyl esters, made with methanol + catalyst.
  • Acyl chlorides (RCOCl) and acid anhydrides ((RCO)2O) react with the four nucleophiles by nucleophilic addition–elimination: + H2O → acid; + alcohol → ester; + 2NH3 → amide; + 2 amine → N-substituted amide.
  • Aspirin (Required practical 10) is made from salicylic acid + ethanoic anhydride — less corrosive, less easily hydrolysed and no HCl formed; purify by recrystallisation and check purity by melting point.

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This topic rewards a clear grasp of the derivatives map and the addition–elimination mechanism: which reagent makes which product, and the arrows for the nucleophile adding then the leaving group departing. Sessions drill acylation and the aspirin synthesis on real AQA past questions.

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Phenylamine behaves exactly like any other primary amine here — its nitrogen lone pair attacks the carbonyl carbon and the product is the N-substituted amide N-phenylethanamide. It is worth knowing by name because it is the aromatic amine AQA use, and because the amide it forms is a solid that can be purified by recrystallisation and identified by its melting point.