Carbon Dioxide → Diazepam

Participants

Reaction Steps

An aqueous solution prepared by dissolving 7 g. of potassium hydroxide in 15 ml. of water is added to an aqueous solution of 3 g. of compound 4306 CB, then 1.8 g. of dimethyl sulphate is gradually added (about 5 minutes) with stirring, care being taken that the temperature does not rise above 25°C. After the addition is ended, the mixture is left for 2 hours at room temperature, then acidified with acetic acid. A pasty product separates which is covered with diisopropyl ether, and the suspension thus formed is heated to boiling for a few minutes; evolution of carbon dioxide takes place. The product is cooled, diluted with ether and the aqueous phase is separated. Upon evaporation of the solvent, there is obtained a residue which is crystallized from diisopropyl ether. Yield: 80%; m.p. 132°C. The product is identical with the product obtained according to Example 16.

Provenance & Evidence