44Carboxylic acids

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ACID CHLORIDES / ACYL CHLORIDES
Definition: RCOCl = carboxylic acid derivative formed by replacement of −OH of −COOH by −Cl
Functional Group: −COCl / acyl chloride group
Nomenclature:
Rule:
Common: −ic acid → −yl chloride
IUPAC: alkanoic acid → alkanoyl chloride
Examples:
    Formula: HCOCl
    Common: Formyl chloride
    IUPAC: Methanoyl chloride
    Formula: CH3COCl
    Common: Acetyl chloride
    IUPAC: Ethanoyl chloride
    Formula: CH3CH2COCl
    Common: Propionyl chloride
    IUPAC: Propanoyl chloride
Preparation:
From Carboxylic Acid:
  1. RCOOH + PCl5 → RCOCl + POCl3 + HCl
  2. 3RCOOH + PCl3 → 3RCOCl + H3PO3
  3. RCOOH + SOCl2 → RCOCl + SO2↑ + HCl↑
Preferred Reagent: SOCl2 → gaseous by-products SO2 + HCl escape → pure acyl chloride
From Salt of Acid:
  1. CH3COONa + PCl3 → CH3COCl + Na3PO3
  2. CH3COONa + PCl5 → CH3COCl + POCl3 + NaCl
  3. CH3COONa + POCl3 → CH3COCl + NaPO3 + NaCl
  4. CH3COONa + SOCl2 → CH3COCl + SO2 + NaCl
Industrial Point: Carboxylate salts cheaper than acids
From Ketene:
  1. CH2=C=O + HCl → CH3COCl
  2. CH3CH=C=O + HCl → CH3CH2COCl
Physical Properties:
State: Lower members → colourless low-boiling liquids; higher members → colourless low-melting solids
Smell: Pungent, irritating
Fuming: RCOCl + H2O → RCOOH + HCl fumes
Solubility: Insoluble in water; soluble in ether, chloroform, acetone, benzene
Boiling Point:
Order: Acid chloride < corresponding carboxylic acid
Reason: No intermolecular H-bonding in acyl chlorides
Examples:
  1. CH3COOH: 391 K > CH3COCl: 324 K
  2. C6H5COOH: 523 K > C6H5COCl: 470 K
Chemical Properties:
Reactivity:
Reason: −Cl has strong −I effect; weak +R effect; acyl carbon strongly electrophilic
Acid Derivative Reactivity Order: RCOCl > (RCO)2O > RCOOR′ > RCONH2
Nucleophilic Acyl Substitution:
Hydrolysis: RCOCl + H2O → RCOOH + HCl
Alcoholysis: RCOCl + R′OH → RCOOR′ + HCl
With Sodium Alkoxide: RCOCl + R′ONa → RCOOR′ + NaCl
Ammonolysis: RCOCl + 2NH3 → RCONH2 + NH4Cl
With 1° Amine: RCOCl + 2R′NH2 → RCONHR′ + R′NH3Cl
With 2° Amine: RCOCl + 2R′2NH → RCONR′2 + R′2NH2Cl
With Carboxylate Salt: RCOCl + R′COONa → RCO−O−COR′ + NaCl
Reduction:
Rosenmund Reduction: RCOCl + H2 / Pd-BaSO4 → RCHO + HCl
LiAlH4: RCOCl → RCH2OH
Organocadmium: RCOCl + R′2Cd → RCOR′
Grignard Reagent: RCOCl + 2R′MgX → tertiary alcohol after hydrolysis
Friedel-Crafts Acylation: Ar−H + RCOCl / anhyd. AlCl3 → ArCOR + HCl
Special Example: C6H6 + CH3COCl / AlCl3 → C6H5COCH3
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ACID ANHYDRIDES
Definition: Acid derivative formed by removal of H2O from two carboxylic acid molecules
General Formula: CnH2n−2O3
Functional Group: RCO−O−COR′
Types:
Simple Anhydride: R = R′
Mixed Anhydride: R ≠ R′
Simplest Theoretical: HCO−O−COH; unstable
Nomenclature:
    Formula: CH3CO−O−COCH3
    Common: Acetic anhydride
    IUPAC: Ethanoic anhydride
    Formula: C2H5CO−O−COC2H5
    Common: Propionic anhydride
    IUPAC: Propanoic anhydride
    Formula: CH3CO−O−COC2H5
    Common: Acetic propionic anhydride
    IUPAC: Ethanoic propanoic anhydride
    Formula: C6H5CO−O−COC6H5
    Common: Benzoic anhydride
    IUPAC: Benzoic anhydride
Preparation:
From Carboxylic Acid: 2RCOOH / P2O5 or heat → RCO−O−COR + H2O
From Dicarboxylic Acids:
Rule: Ortho dicarboxylic acids or suitable dicarboxylic acids lose H2O intramolecularly
Example: Phthalic acid → phthalic anhydride + H2O
Lab Method: RCOCl + RCOONa / anhydrous → RCO−O−COR + NaCl
Example: CH3COCl + CH3COONa → (CH3CO)2O + NaCl
Physical Properties:
State: Lower aliphatic anhydrides → colourless liquids; higher/aromatic anhydrides → solids
Smell: Pungent
Solubility: Insoluble in water; soluble in alcohol, ether, acetone
Boiling Point:
Order: Acid anhydride > corresponding carboxylic acid
Reason: Greater molecular mass → stronger Van der Waals forces
Example: Acetic acid: 391 K < acetic anhydride: 413 K
Chemical Properties:
Acylating Nature: Less vigorous than acid chloride; easily controlled
Hydrolysis:
Reaction: RCO−O−COR + H2O → 2RCOOH
Rate Order: Alkaline > acidic > neutral
Alcoholysis: RCO−O−COR + R′OH → RCOOR′ + RCOOH
Example Alcoholysis: (CH3CO)2O + C2H5OH → CH3COOC2H5 + CH3COOH
Ammonolysis: RCO−O−COR + NH3 → RCONH2 + RCOOH
Example Ammonolysis: (CH3CO)2O + NH3 → CH3CONH2 + CH3COOH
With Amines: RCO−O−COR + R′NH2 → RCONHR′ + RCOOH
Reduction: (RCO)2O + LiAlH4 → 2RCH2OH
With PCl5: (RCO)2O + PCl5 → 2RCOCl + POCl3
With SOCl2: (RCO)2O + SOCl2 → 2RCOCl + SO2
With HX: RCO−O−COR + HX → RCOX + RCOOH
With Acetaldehyde: (CH3CO)2O + CH3CHO → CH3CH(OCOCH3)2
Friedel-Crafts Acylation:
General: Ar−H + (RCO)2O / anhyd. AlCl3 → ArCOR + RCOOH
Example: C6H6 + (CH3CO)2O / AlCl3 → C6H5COCH3 + CH3COOH
Dicarboxylic Anhydrides: Readily give keto acids in Friedel-Crafts acylation
Uses:
  1. Acylating agent for alcohols, phenols, amines
  2. Detection/estimation of −OH and −NH2 groups
  3. Manufacture of aspirin
  4. Manufacture of acetophenone
  5. Manufacture of acetamide
  6. Manufacture of cellulose acetate
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ACID AMIDES
Definition: Carboxylic acid derivatives formed by replacement of −OH of −COOH by −NH2, −NHR or −NR2
General Formula: CnH2n+1NO
Types:
    Type: Primary amide
    Formula: RCONH2
    Type: Secondary amide
    Formula: RCONHR′
    Type: Tertiary amide
    Formula: RCONR′2
Preparation:
From Carboxylic Acid:
  1. RCOOH + NH3 → RCOO−NH4+
  2. RCOO−NH4+ / Δ → RCONH2 + H2O
Example: CH3COOH + NH3 → CH3COONH4 → CH3CONH2 + H2O
Ammonolysis of Acid Chloride: RCOCl + 2NH3 → RCONH2 + NH4Cl
Ammonolysis of Acid Anhydride: (RCO)2O + NH3 → RCONH2 + RCOOH
Ammonolysis of Ester: RCOOR′ + NH3 → RCONH2 + R′OH
Partial Hydrolysis of Nitrile: RCN + H2O / acid or alkaline H2O2 → RCONH2
From Urea: RCOOH + NH2CONH2 / Δ → RCONH2 + CO2 + NH3
Physical Properties:
State: Formamide → liquid; other amides → colourless crystalline solids
Solubility: Lower aliphatic amides up to C6 soluble in water; higher/aromatic amides insoluble
Reason for Solubility: Intermolecular H-bonding with water
Melting/Boiling Point:
High: Strong intermolecular H-bonding
Order: Amide > corresponding carboxylic acid
Examples:
  1. Acetamide: 494 K > acetic acid: 391 K
  2. Benzamide: 563 K > benzoic acid: 523 K
Chemical Properties:
Reactivity:
Order: Least reactive acid derivative
Reason: Strong +R effect of −NH2 decreases electrophilicity of carbonyl carbon
Amphoteric Nature:
Nature: Very weak acid + very weak base
Litmus: No effect
Acidic Character: 2RCONH2 + 2Na → 2RCONHNa + H2↑
Basic Character: RCONH2 + HCl → RCONH2·HCl
Hydrolysis:
Acidic: RCONH2 + H2O + HCl → RCOOH + NH4Cl
Alkaline: RCONH2 + NaOH → RCOONa + NH3
Dehydration:
Reagents: P2O5, SOCl2, POCl3
Reaction: RCONH2 → RCN + H2O
Reduction:
LiAlH4: RCONH2 → RCH2NH2
Meaning: Amide → 1° amine
Hofmann Bromamide Degradation:
Reaction: RCONH2 + Br2 + 4KOH → RNH2 + K2CO3 + 2KBr + 2H2O
Product: 1° amine with one carbon less
Key: Carbonyl carbon removed as carbonate
With Nitrous Acid: RCONH2 + HNO2 → RCOOH + N2 + H2O
With Grignard Reagent:
Primary/Secondary Amide: Acidic N−H reacts with RMgX → hydrocarbon + magnesium salt
Tertiary Amide: RCONR′2 + RMgX → ketone after hydrolysis
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ACID DERIVATIVES: HIGH-YIELD COMPARISON
General Derivative Pattern: RCO−Z
Leaving Group Strength: Cl− > RCOO− > RO− > NH2−
Reactivity Order: Acid chloride > Acid anhydride > Ester > Amide
Common Reaction Type: Nucleophilic acyl substitution
Boiling Point Trend:
Acid Chloride: Lower than acid; no H-bonding
Ester: Lower than acid; no self H-bonding
Acid Anhydride: Higher than acid; larger molecular size
Amide: Highest; strong H-bonding
Hydrolysis Products:
    Derivative: RCOCl
    Product: RCOOH + HCl
    Derivative: (RCO)2O
    Product: 2RCOOH
    Derivative: RCOOR′
    Product: RCOOH + R′OH / acid; RCOO− + R′OH / base
    Derivative: RCONH2
    Product: RCOOH + NH4+ / acid; RCOO− + NH3 / base
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READ AND DIGEST
  1. Sodium benzoate → food preservative
  2. Formamide → liquid; other amides → crystalline solids
  3. Alkaline K2Cr2O7 not used for oxidation of 1° alcohols/aldehydes because K2CrO4 forms
  4. Formic acid lab preparation: glycerol + hydrated oxalic acid at 110°C
  5. Esterification reactivity decreases with steric hindrance
  6. Alcohol reactivity: CH3OH > CH3CH2OH > (CH3)2CHOH
  7. Acid reactivity: HCOOH > CH3COOH > (CH3)2CHCOOH
  8. β-keto acids and β-dicarboxylic acids decarboxylate readily on heating
  9. 100% acetic acid = glacial acetic acid; m.p. 289.6 K
  10. Sucrose + conc. HNO3 → oxalic acid
  11. Carboxylic acids do not show usual carbonyl reactions due to resonance with −OH
  12. CuO·CuCr2O4 = copper chromite = Adkins catalyst
  13. Formic acid reduces Tollens reagent, Fehling solution, HgCl2 and KMnO4
  14. Sodium formate + soda lime → H2
  15. Sodium formate on heating → sodium oxalate
  16. Cream of tartar = potassium hydrogen tartrate; used in baking powder
  17. Glacial acetic acid appears ice-like below 16.6°C
Q1.
In the following chain of reactions, what is the product C? (start: CH₃COOH → … → C) [IOM 2006]
📅IOM 2006
Q2.
An organic compound 'A' on treatment with silver nitrate followed by acid hydrolysis gives acetic acid. The compound 'A' is.
📅IOM 2004
Q3.
The product of acylation is
📅IOM 2002
Q4.
Acetyl salicylic acid (Aspirin) acts as
📅KU 2008MOE 2008
Q5.
Aspirin is
Q6.
Which of the following compound is Aspirin?
📅MOE 2062
Q7.
Formic acid is formed by
📅MOE 2056
Q8.
Which of the following acids do not contain a carboxyl group?
Q9.
The catalyst used in the hydrogenation of oil is
📅MOE
Q10.
The reaction of formic acid with conc. H₂SO₄ gives
📅MOE
Q11.
The reaction CH₃COOH + C₂H₅OH → CH₃COOC₂H₅ + H₂O is an example of
📅MOE
Q12.
Acetamide will form methyl amine when treated with:
📅MOE
Q13.
Formic acid is prepared in the lab by
📅MOE
Q14.
The acid which reduces Fehling's solution is
📅BPKIHS
Q15.
The general formula (RCO)₂O represents
📅LE/K.U.
Q16.
Acetamide is