反应详情

A mixture of 7 g. of 4,9-dihydro-9-methyl-10H-thieno[3,4-b][1,5]benzodiazepin-10-one and 4.6 g. (4.8 ml.) of hexanoyl chloride in 70 ml. of benzene is heated with stirring under reflux for 3 hours. The reaction mixture is stirred with cooling in an ice bath for 2 hours, 150 ml. of hexane is added and the mixture is placed in a chill room. The solvents are removed in vacuo on a steam bath. A 10 ml. portion of ether is added to the residue and the mixture is returned to the chill room. The tan crystals are collected by filtration, washed with ether and dried. The ether is concentrated giving a green oil which is triturated twice with hexane and once with a mixture of hexane and ether, giving crystals which are collected, washed with ether and dried. The two crops of crystals are combined, dissolved with warming in 75 ml. of ether and filtered. The filtrate is concentrated to 35 ml. and stored in a cold room for 4 hours. The solid is collected, washed with ether then hexane and dried, giving the desired product, mp. 76°-77° C.

1. additionA mixture of 7 g
2. temperatureunder reflux for 3 hours
3. stirringThe reaction mixture is stirred
4. temperaturewith cooling in an ice bath for 2 hours
5. customThe solvents are removed in vacuo on a steam bath
6. additionportion of ether is added to the residue
7. filtrationThe tan crystals are collected by filtration
8. washwashed with ether
9. customdried
10. concentrationThe ether is concentrated
11. customgiving a green oil which
12. customis triturated twice with hexane and once with a mixture of hexane and ether
13. customgiving crystals which
14. customare collected
15. washwashed with ether
16. customdried
17. dissolutiondissolved
18. temperaturewith warming in 75 ml
19. filtrationof ether and filtered
20. concentrationThe filtrate is concentrated to 35 ml
21. customThe solid is collected
22. washwashed with ether
23. dry with materialhexane and dried