反应详情

On a water-bath kept at 14° C., to a solution of (3aR*,10aS*)-9-benzyl-2,3,3a,4,9,10a-hexahydrobenzo[b]cyclopenta[e][1,4]diazepin-10(1H)-one (5.85 g, 20 mmol) in 1,2-dichloroethane (20 mL) was added dropwise a solution of chloroacetyl chloride (2.5 g, 22 mmol) in 1,2-dichloroethane (15 mL), and the mixture was stirred for 10 minutes. The aqueous layer of this mixture was separated, and the organic layer was washed with water and a saturated aqueous solution of sodium chloride, dried over magnesium sulfate, which was subjected to filtration, and the filtrate was concentrated under reduced pressure. The concentrate was recrystallized from dichloromethane-hexane to give 6.49 g (yield 88%) of the titled compound, m.p. 154°-156° C.

1. customThe aqueous layer of this mixture was separated
2. washthe organic layer was washed with water
3. dry with materiala saturated aqueous solution of sodium chloride, dried over magnesium sulfate, which
4. filtrationwas subjected to filtration
5. concentrationthe filtrate was concentrated under reduced pressure
6. customThe concentrate was recrystallized from dichloromethane-hexane