Potassium Hydroxide → 7-Chloro-4-methyl-10-(methylthio)-4H-thieno[3,4-b][1,5]benzodiazepine

Participants

Reaction Steps

To a stirred suspension of 1.1 g. of 7-chloro-4-methyl-4,9-dihydro-10H-thieno[3,4-b][1,5]benzodiazepin-10-thione in 15 ml. of dioxane is added dropwise and simultaneously at 30°-40° C., a solution of 1.3 g. of potassium hydroxide in 15 ml. of methanol and 1.1 g. of methyl sulfate. After addition is complete, the mixture is stirred for 3 hours, diluted with methanol and filtered. The filtrate is concentrated to 20 ml., diluted with water and the precipitate is collected. Recrystallization from methanol-water gives deep yellow crystals, m.p. 156°-158° C.

Provenance & Evidence