反应详情

To a stirred suspension of 0.7 g. of 4,9-dihydro-4-methyl-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 ml. of methyl sulfate. After addition is complete the mixture is stirred for 3 hours, diluted with methanol and filtered. The filtrate is concentrated to about 20 ml., diluted with water and extracted with chloroform. The chloroform solution is concentrated to give a solid, which is recrystallized from methanol-water to give orgnae crystals, m.p. 113°-115° C.

1. additionTo a stirred suspension of 0.7 g
2. additionAfter addition
3. filtrationfiltered
4. concentrationThe filtrate is concentrated to about 20 ml
5. addition, diluted with water
6. extractionextracted with chloroform
7. concentrationThe chloroform solution is concentrated
8. customto give a solid, which
9. customis recrystallized from methanol-water
10. customto give orgnae crystals, m.p. 113°-115° C.