反应详情

温度

-78 °C

To a solution of 4,4-difluoro-N-methyl cyclohexanecarboxamide (3 g, 14.5 mmol) in THF (20 mL) were added CH3MgBr (5.19 g, 43.5 mmol) in −78° C. The mixture was stirred at −78° C. for 5 hr. Water (10 mL) was added and the mixture was concentrated and extracted by CH2Cl2 (40 mL*3). The organic layer was washed with brine and dried over sodium sulfate. The organic layer was concentrated to give 1-(4,4-difluorocyclohexyl)ethanone (1.5 g, crude) for next step.

1. concentrationthe mixture was concentrated
2. extractionextracted by CH2Cl2 (40 mL*3)
3. washThe organic layer was washed with brine
4. dry with materialdried over sodium sulfate
5. concentrationThe organic layer was concentrated