Water → 2,4-Dibromo-N-methylbutanamide

Participants

Reaction Conditions

Reaction Steps

A solution mixture consisting of 40% aqueous methylamine solution (7.9 g, 0.10 mol, manufactured by JUNSEI CHEMICAL CO., LTD.) and water (3.3 g) was cooled to not more than 10° C. To the solution mixture, 2,4-dibromobutyric acid bromide (38 g, 0.12 mol) was added dropwise over a period of 15 minutes while keeping the temperature at not more than 10° C. After the completion of the dropwise addition, the mixture was heated to 30° C. and stirred for 30 minutes. The reaction liquid was combined with 50 g of chloroform, and the organic phase was extracted. The organic phase was separated and dried over magnesium sulfate, and the magnesium sulfate was filtered out. The organic phase obtained was concentrated to afford a crude crystal, which was then washed with a 1:1 solution of diethyl ether and hexane to give N-methyl-2,4-dibromobutyric acid amide (21.4 g, 0.083 mol, mp: 54° C., yield: 69%).

Provenance & Evidence