反应详情

NCS (3.14 g. 23.5 mmol) was added to a solution of N-(4-chloropyridin-2-yl)pivalamide (1.00 g, 4.7 mmol) in dry acetonitrile (10 mL). The resulting suspension was heated for 3 h and then cooled to r.t. The solvent was removed in vacuo and the crude mixture was diluted with ethyl acetate (50 mL). The organic phase was washed with aqueous NaOH (10%, 2×20 mL), water (20 mL) and dried (MgSO4). The solvent was removed in vacuo and the crude mixture was purified by flash chromatography on silica, eluting with ethyl acetate and hexane (1/9), to give the title compound as a colourless solid (0.87 g, 75%).

1. temperatureThe resulting suspension was heated for 3 h
2. customThe solvent was removed in vacuo
3. additionthe crude mixture was diluted with ethyl acetate (50 mL)
4. washThe organic phase was washed with aqueous NaOH (10%, 2×20 mL), water (20 mL)
5. dry with materialdried (MgSO4)
6. customThe solvent was removed in vacuo
7. customthe crude mixture was purified by flash chromatography on silica
8. washeluting with ethyl acetate and hexane (1/9)