反应详情

温度

-78 °C

To a solution of tert-butyl 2-(methoxy(methyl)carbamoyl)morpholine-4-carboxylate (11 g, 4.0 mmol) in THF (40 mL) was added CH3MgBr (4 mL, 12 mmol) at −78° C. The mixture was stirred at −78° C. for 3 hr. Water (20 mL) was added and the mixture was extracted by ethyl acetate (80 mL*3). The organic layer was washed with brine and dried over sodium sulfate. The crude product was concentrated and purified by column chromatography on silica gel (eluted: petroleum ether/ethyl acetate=10/1) to give tert-butyl 2-acetylmorpholine-4-carboxylate (8 g, 86%).

1. extractionthe mixture was extracted by ethyl acetate (80 mL*3)
2. washThe organic layer was washed with brine
3. dry with materialdried over sodium sulfate
4. concentrationThe crude product was concentrated
5. custompurified by column chromatography on silica gel (eluted: petroleum ether/ethyl acetate=10/1)