反应详情

7-t-Butoxycarbonylamino-4-oxo-7-methyl-5-azaspiro[2.4]heptane (42.63 g) was suspended in dimethylformamide (850 mL) under a nitrogen gas atmosphere, and the suspension was cooled with ice. To the suspension, 60% sodium hydride (6.93 g) was added, and the mixture was returned to room temperature. Subsequently, benzyl bromide (22.64 mL) was added to the reaction mixture, followed by stirring. After three hours, insoluble material was removed through filtration, and water was added to the filtrate. Ethyl acetate was further added thereto for extraction. The organic layer obtained through extraction was dried with sodium sulfate, followed by filtration. The filtrate was concentrated under reduced pressure, to thereby yield an oily residue. The residue was subjected to silica gel chromatography (hexane:ethyl acetate), to thereby yield the title product as pale yellow oil (51.0 g, yield: 89.2%).

1. temperaturethe suspension was cooled with ice
2. customwas returned to room temperature
3. custominsoluble material was removed through filtration, and water
4. additionwas added to the filtrate
5. additionEthyl acetate was further added
6. extractionfor extraction
7. customThe organic layer obtained through extraction
8. dry with materialwas dried with sodium sulfate
9. filtrationfollowed by filtration
10. concentrationThe filtrate was concentrated under reduced pressure
11. customto thereby yield an oily residue