反应详情

To a solution of 4,4-difluoropiperidine hydrochloride (1.44 g, 9 mmol) in DCM (15 mL) was added chloroacetic acid (0.94 g, 10 mmol), TEA (1.5 mL), EDC (3.82 g, 20 mmol) and DMAP (cat.). The reaction mixture was stirred at RT overnight. The contents were transferred to a separatory funnel and DCM layer was washed saturated NaHCO3 solution, dried over anhydrous Na2SO4. The crude product was purified by flash column chromatography using 3:1 Pet. Ether:DCM in. 2-(4,4-difluoropiperidin-1-yl)acetyl chloride was isolated as a white solid weighing 1.57 g (yield: 88%).

1. customThe contents were transferred to a separatory funnel
2. washDCM layer was washed saturated NaHCO3 solution
3. dry with materialdried over anhydrous Na2SO4
4. customThe crude product was purified by flash column chromatography