反应详情

To a stirred suspension of 0.8 g. of 7-chloro-4,9-dihydro-10H-thieno[3,4-b] [1,5] benzodiazepine-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 methyl sulfate. After addition is complete, the reaction mixture is stirred for 3 hours, diluted with methanol and filtered. The filtrate is concentrated to 20 ml., diluted with water and extracted with chloroform. The chloroform solution is concentrated under reduced pressure to give a solid, which is recrystallized from methanol-water to give yellow crystals, m.p. 111°-113°C.

1. additionTo a stirred suspension of 0.8 g
2. additionAfter addition
3. filtrationfiltered
4. concentrationThe filtrate is concentrated to 20 ml
5. addition, diluted with water
6. extractionextracted with chloroform
7. concentrationThe chloroform solution is concentrated under reduced pressure
8. customto give a solid, which
9. customis recrystallized from methanol-water
10. customto give yellow crystals, m.p. 111°-113°C.