反应详情

4-(Benzyloxycarbonyl)-2-piperazinone (4.685 g) was dissolved in DMF (170 ml) and combined with sodium hydride (800 mg, in oil) with cooling on ice. After stirring at room temperature for 30 minutes, O-diphenylphosphinyl hydroxylamine (4.896 g) was added and the mixture was stirred at 50° C. for 15 hours. The reaction mixture was concentrated under reduced pressure, and the residue was combined with aqueous sodium bicarbonate and extracted with dichloromethane. The extract was dried and concentrated to obtain the title compound 1-amino-4-benzyloxycarbonyl-2-piperazinone (4.8 g) as a colorless oil.

1. temperaturewith cooling on ice
2. stirringthe mixture was stirred at 50° C. for 15 hours
3. concentrationThe reaction mixture was concentrated under reduced pressure
4. extractionextracted with dichloromethane
5. customThe extract was dried
6. concentrationconcentrated