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Chapter 19: Carbonyl Compounds III

Learning Objectives:

1. Write the mechanism for keto- tautomerization and explain the consequence of such tautomerizarion in the optical chiral of compound. 2. Remember the approximate p Ka value for the α-hydrogen of a . 3. Provide appropriate bases for the formation of and use such enolate for halogenation and alkylation. 4. Be able to write the general electron-pushing (arrow-pushing) mechanisms of , , , and Dieckmann condensation. 5. Be able to write the general electron-pushing (arrow-pushing) mechanisms for of 3-oxocarboxylic acids 6. Be able to employ the above-mentioned reaction for the formation of new carbon-carbon bond

Sections:

19.1 Acidity of α-hydrogens* 19.2 Keto-Enol Tautomerism* 19.3 How and Enolate Ions React* 19.4 Halogenation of the α-Carbon of and * 19.5 Halogenation of the α-Carbon of Carboxylic Acids: The Hell-Volhard-Zelinski (HVZ) Reaction 19.6 α-Halogenated Carbonyl Compounds in Synthesis* 19.7 Using LDA to form an Enolate* 19.8 Alkylation of the α-Carbon of Carbonyl Compounds* 19.9 Alkylation and Acylation of the α-Carbon via an Intermediate 19.10 Alkylation of the β-Carbon: the Michael Reaction* 19.11 The Aldol Reaction* 19.12 Dehydration of Aldol Addition Products: Formation of α,β -Unsaturated Aldehydes and Ketones* 19.13 The Mixed Aldol Reaction 19.14 The Claisen Condensation* 19.15 The Mixed Claisen Condensation 19.16 Intramolecular Condensation and Addition Reactions* 19.17 Decarboxylation of 3-Oxocarboxylic Acids* 19.18 The Malonic Synthesis: Synthesis of Carboxylic Acids 19.19 The Acetoacetic Ester Synthesis: Synthesis of Methyl Ketones 19.20 Designing a Synthesis VI: Making New Carbon-Carbon Bonds 19.21 Reactions at the α-carbon in Biological Systems #

* Sections that will be focused # Sections that will be skipped

Recommended additional problems

19.44 – 19.52, 19.54 – 19.64, 19.66 – 19.80

1 Class Note

19.1 Acidity of α-hydrogens

A. pKa of α-hydrogen of carbonyl derivatives

O O O O R' α R' R' R' NHR OR R H H H H H

O O O O O O

R' OR R' R R' H H H H

B. effect

2 19.2 Keto-Enol Tautomerism

O OH R' R R' R H

A. Mechanism in acidic condition

B. Mechanism in basic condition

3 19.3 How Enols and Enolate Ions React

A. Analysis of enols and

4 19.4 Halogenation of the α-Carbon of Aldehydes and Ketones

A. Acid-catalyzed halogenation

O O X2 (Cl2, Br2, I2) + H3O CH3 CH2 X

5 B. -promoted halogenation

O X2 (Cl2, Br2, I2) O (excess) R HO- R CH2 CX2

C. Haloform reaction

O X2 (Cl2, Br2, I2) O (excess) HO- CH O 3 + CHX3

6 19.5 Halogenation of the α-Carbon of Carboxylic Acids: The Hell-Volhard-Zelinski (HVZ) Reaction

1) PBr , Br O 3 2 O 2) H2O R R OH OH Br

7 19.6 α-Halogenated Carbonyl Compounds in Synthesis

A. Analysis of α-halogenated carbonyl Compounds

B. Examples

8 19.7 Using LDA to form an Enolate

N

diisopropylamide (LDA)

19.8 Alkylation of the α-Carbon of Carbonyl Compounds

A. Analysis of the reaction

9 B. Examples

(i) 1) LDA, THF OCH3 2) CH3I

O

(ii) 1) LDA, THF 2) CH3CH2I CN

10 C. Potential problem in alkylation of the α-carbon of carbonyl compounds

O 1) LDA, THF CH3 2) CH3I

11 19.9 Alkylation and Acylation of the α-Carbon via an Enamine Intermediate

O N catalytic H+

+ N H2O H + pyrrolidine enamine

A. Examples 1) catalytic H+

O N H

2) CH3Br + 3) H2O, H

12 19.10 Alkylation of the β-Carbon: the Michael Reaction

A. Michael reaction

O O O - CH3O + CH CH 3 H3C 3

13 B. Examples

(i) O O O base (?)

+ H3CO OCH3

(ii) O O base (?) CN OCH CH + 2 3 H3C

14 C. Stork enamine reaction

O N HCl H2O + CH3

15 19.11 The Aldol Reaction

OH O O base R R H H R

A. Mechanism

16 19.12 Dehydration of Aldol Addition Products: Formation of α,β -Unsaturated Aldehydes and Ketones

A.

B. Examples

(i) O O - H MeO + H MeOH

(ii) O EtO- Na+

EtOH

17 19.13 The Mixed Aldol Reaction

A. Potential problem in aldol reaction

(i) O EtO- Na+

EtOH

(ii) O O MeO- Na+ + MeOH H

18 B. Solution

(i) O O - + H MeO Na + H MeOH

19 19.14 The Claisen Condensation and 19.15 The Mixed Claisen Condensation

O O O base R R OR' + HOR' OR' R

A. Mechanism

20 B. Examples

(i) O base (?) OCH2CH3

(ii) O O base (?) OCH3 + OCH2CH3

21 19.16 Intramolecular Condensation and Addition Reactions

A. Intramolecular Claisen reaction (Dieckmann condensation)

(i) H3CO OCH3 MeO- Na+ MeOH O O

(ii) O

EtO- Na+ H3CH2CO OCH2CH3 EtOH

O

22 B. Intramolecular aldol reaction

(i) H3C CH3 MeO- Na+ MeOH O O

(ii) O

EtO- Na+ H3C CH3 EtOH

O

23 (iii) O

EtO- Na+ H3C H EtOH

O

(iv)

O O + base H , heat + + H2O CH3 O

24 19.17 Decarboxylation of 3-Oxocarboxylic Acids

A. Easier in acidic condition: mechanism

O O O O

R OH R O

B. Examples of compounds containing 3-oxocarboxylic acid

O O O O

HO OH OH

R R

25 19.18 The : Synthesis of Carboxylic Acids and 19.19 The Acetoacetic Ester Synthesis: Synthesis of Methyl Ketones

O O O ? R H3CH2CO OCH2CH3 OH

26 A. Examples:

O O O

OH OH OH

27 19.20 Designing a Synthesis VI: Making New Carbon-Carbon Bonds

O O CO2H synthesis of from H3CO OCH3

28