反应详情

温度

0 °C

Tert-butyl 3-(methoxy(methyl)carbamoyl)piperidine-1-carboxylate (8.17 g, 30 mmol) was dissolved in THF (100 mL) and cooled to 0° C., methylmagnesium bromide (3.0 M in Et2O, 11 mL, 33 mmol) was added dropwise. The reaction mixture was warmed to room temperature and stirred overnight. After quench with saturated NH4Cl, the reaction mixture was extracted with EtOAc, dried and concentrated. The crude product was column purified with mixture of hexane and EtOAc to give tert-butyl 3-acetylpiperidine-1-carboxylate (4.8 g).

1. temperatureThe reaction mixture was warmed to room temperature
2. customAfter quench with saturated NH4Cl
3. extractionthe reaction mixture was extracted with EtOAc
4. customdried
5. concentrationconcentrated
6. custompurified with mixture of hexane and EtOAc