反应详情

A reaction mixture comprising 7 g. of 4,9-dihydro-9-methyl-10H-thieno[3,4-b][1,5]benzodiazepin-10-one, 3.1 g. (2.9 ml.) of propionyl chloride and 70 ml. of benzene is refluxed for 3 hours and then allowed to stand for 48 hours. The benzene is distilled off. The residue is filtered, washed with ether and dried. The solid is heated to boiling in 300 ml. of ethyl acetate, filtered and the filtrate is chilled. The crystals are collected, washed with ether and dried giving the desired product, mp. 202°-203° C.

1. distillationThe benzene is distilled off
2. filtrationThe residue is filtered
3. washwashed with ether
4. customdried
5. temperatureThe solid is heated
6. filtrationof ethyl acetate, filtered
7. temperaturethe filtrate is chilled
8. customThe crystals are collected
9. washwashed with ether
10. customdried