Potassium Hydroxide → HCID 12521661, compound

Participants

Reaction Steps

To a stirred suspension of 0.7 g. of 6-chloro-4,9-dihydro-10H-thieno[3,4-b] [1,5]benzodiazepin-10-thione in 10 ml. of dioxane is added dropwise and simultaneously at 30°-40°C., a solution of 0.95 g. of potassium hydroxide in 10 ml. of methanol and 0.8 g. of methylsulfate. After addition is complete, the mixture is stirred for 3 hours, diluted with methanol and filtered. The filtrate is concentrated to 20 ml. and diluted with water. The precipitate is collected, washed with water and recrystallized from methanol-water to give yellow crystals, m.p. 152°-154°C.

Provenance & Evidence