Conjugate Carbonyl Additions: The Michael Reaction

23.10 Conjugate Carbonyl Additions: The Michael Reaction

23.10 • Conjugate Carbonyl Additions: The Michael Reaction

We saw in Section 19.13 that certain nucleophiles, such as amines, react with α,β-unsaturated aldehydes and ketones to give a conjugate addition product, rather than a direct addition product.

The reversible reaction shows a conjugated carbonyl compound reacting with a nucleophile to form an intermediate with a carbanion. Further reaction of intermediate yields a conjugate addition product.

Exactly the same kind of conjugate addition can occur when a nucleophilic enolate ion reacts with an α,β-unsaturated carbonyl compound—a process known as the Michael reaction after Arthur Michael at Tufts College and Harvard University.

The best Michael reactions are those that take place when a particularly stable enolate ion, such as that derived from a β-keto ester or other 1,3-dicarbonyl compound, adds to an unhindered α,β-unsaturated ketone. For example, ethyl acetoacetate reacts with 3-buten-2-one in the presence of sodium ethoxide to yield the conjugate addition product.

The reaction of ethyl acetoacetate with 3-buten-2-one with sodium ethoxide in ethanol, then hydronium ion, forms a conjugate addition product with an extended carbon chain.

Michael reactions take place by addition of a nucleophilic enolate ion donor to the β carbon of an α,β-unsaturated carbonyl acceptor, according to the mechanism shown in Figure 23.7.

Figure 23.7 MECHANISM
Mechanism of the Michael reaction between a β-keto ester and an α,β-unsaturated ketone. The reaction is a conjugate addition of an enolate ion to the unsaturated carbonyl compound.
An arrow-pushing mechanism of the Michael reaction of ethyl-3-oxobutanoate involving three steps. These are proton abstraction, formation of an enolate, and product formation.

The Michael reaction occurs with a variety of α,β-unsaturated carbonyl compounds, not just conjugated ketones. Unsaturated aldehydes, esters, thioesters, nitriles, amides, and nitro compounds can all act as the electrophilic acceptor component in Michael reactions (Table 23.1). Similarly, a variety of different donors can be used, including β-diketones, β-keto esters, malonic esters, β-keto nitriles, and nitro compounds.

Table 23.1 Some Michael Acceptors and Michael Donors
Michael acceptors Michael donors
The structure of the propenal shows a three-carbon chain. A double bond is shared between the second and third carbon. The first carbon is part of C H O group. Propenal The structure of beta-diketone, a Michael donor. Carbonyl with substituent R is bonded to C H 2, which is bonded to another carbonyl with substituent R prime. β-Diketone
The structure of but-3-en-2-one (Michael acceptor) shows a four-carbon chain with a carbonyl at the second carbon. A double bond connects the third and fourth carbon. 3-Buten-2-one The beta-keto ester has a C H 2 group between two carbonyls. An ethoxy group is attached to one terminal carbonyl, and an R group is on the other terminus. β-Keto ester
The structure of ethyl propenoate (Michael acceptor) shows a three-carbon chain where the second and third carbon share double bond. An ethoxy group is attached to the first carbonyl carbon. Ethyl propenoate The structure of diethyl malonate, a Michael donor. Carbonyl with ethoxy substituent is bonded to C H 2, which is bonded to another carbonyl with ethoxy substituent. Diethyl malonate
The structure of propenamide (Michael acceptor) shows a three-carbon chain with N H 2 group attached to the carbonyl carbon. The second and third carbon atoms are double-bonded. Propenamide The structure of beta-keto nitrile, Michael donor. R is bonded to the carbonyl group which is further bonded to methylene. Methylene is bonded with a cyanide group. β-Keto nitrile
The structure of propenenitrile (acrylonitrile) shows a three-carbon chain where the first carbon is triple-bonded to nitrogen. A double bond is shared between the second and third carbon atoms. Propenenitrile The structure of a nitro compound, Michael-donor. R group is single-bonded to methylene which is further linked to the nitro group. Nitro compound
The structure of nitroethylene (Michael acceptor) shows a two-carbon chain. N O 2 group is attached to the first carbon. The first and second carbon atoms are double-bonded. Nitroethylene

Worked Example 23.5

Using the Michael Reaction

How might you obtain the following compound using a Michael reaction?

The structure shows a cyclohexanone ring connected to C O O E t and C H 2 C H 2 C O O E t groups at the first carbon.

Strategy

A Michael reaction involves the conjugate addition of a stable enolate ion donor to an α,β-unsaturated carbonyl acceptor, yielding a 1,5-dicarbonyl product. Usually, the stable enolate ion is derived from a β-diketone, β-keto ester, malonic ester, or similar compound. The C–C bond formed in the conjugate addition step is the one between the α carbon of the acidic donor and the β carbon of the unsaturated acceptor.

Solution

The reaction between ethyl-2-oxocyclohexanecarboxylate with alpha, beta-unsaturated ester (three-carbon) in the presence of sodium ethoxide in ethanol gives ethyl-1-(3-ethoxy-3-oxopropyl)-2-oxocyclohexanecarboxylate (1,5-dicarbonyl compound) with a new carbon-carbon bond between cyclohexane and ester.
Problem 23-16
What product would you obtain from a base-catalyzed Michael reaction of 2,4-pentanedione with each of the following α,β-unsaturated acceptors?
(a)
2-Cyclohexenone
(b)
Propenenitrile
(c)
Ethyl 2-butenoate
Problem 23-17
What product would you obtain from a base-catalyzed Michael reaction of 3-buten-2-one with each of the following nucleophilic donors?
(a)
Structure of diethyl malonate, a 3-carbon chain with ethy esters on the terminal carbons.
(b)
Structure of cyclopentanone with C O O E t on C 2.
Problem 23-18

How would you prepare the following compound using a Michael reaction (gray = H, black = C, red = O, blue = N)?

The ball-and-stick model shows a seven-carbon chain with N O 2 on sixth and carbonyl on third carbons. Gray, white, red, and blue spheres denote carbon, hydrogen, oxygen, and nitrogen.