反应详情

A mixture of tert-butyl piperazine-1-carboxylate (6.2 g, 33.29 mmol), epibromohydrin (5.4 g, 39.42 mmol) and potassium carbonate (5.5 g, 39.79 mmol) in acetonitrile (70 ml) was heated under reflux for 3 hours. The reaction mixture was concentrated under reduced pressure, and water was added to the residue. The mixture was extracted with methylene chloride. The extract was washed with brine, dried over sodium sulfate, and then filtered, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate) to afford tert-butyl 4-oxiranylmethylpiperazine-1-carboxylate (6.2 g, yield 77%) as a colorless oil.

1. temperaturewas heated
2. temperatureunder reflux for 3 hours
3. concentrationThe reaction mixture was concentrated under reduced pressure, and water
4. additionwas added to the residue
5. extractionThe mixture was extracted with methylene chloride
6. washThe extract was washed with brine
7. dry with materialdried over sodium sulfate
8. filtrationfiltered
9. concentrationthe filtrate was concentrated under reduced pressure
10. customThe residue was purified by silica gel column chromatography (ethyl acetate)