反应详情

A suspension of (3aR*,10aS*)-9-benzyl-4-(phthalimidoacetyl)-2,3,3a,4,9,10a-hexahydrobenzo[b]cyclopenta[e][1,4]diazepin-10(1H)-one (9.82 g, 20 mmol) and hydrazine monohydrate (2.31 g, 46 mmol) in ethanol (200 mL) was refluxed for 3.5 hours. The reaction mixture was cooled, which was subjected to filtration. The filtrate was washed with chloroform, which was concentrated under reduced pressure. The concentrate was suspended in chloroform, which was again subjected to filtration. The filtrate was concentrated under reduced pressure. The concentrate was crystallized from dichloromethane-hexane to give 5.62 g (yield 80%). The sample for analytical experiment was prepared by recrystallization from dichloromethane-diisopropylether. m.p. 163°-165° C.

1. temperaturewas refluxed for 3.5 hours
2. temperatureThe reaction mixture was cooled
3. filtrationwhich was subjected to filtration
4. washThe filtrate was washed with chloroform, which
5. concentrationwas concentrated under reduced pressure
6. filtrationwhich was again subjected to filtration
7. concentrationThe filtrate was concentrated under reduced pressure
8. customThe concentrate was crystallized from dichloromethane-hexane
9. customto give 5.62 g (yield 80%)