反应详情

温度

0 °C

To a solution of N-cyclopropyl-N-piperidin-4-yl-3-trifluoromethyl-benzene sulfonamide (1045 mg, 3 mmol) in CH2Cl2 was added triethylamine (0.418 ml, 3 mmmol) and acryloyl chloride (0.244 ml, 3 mmol) at 0° C. The reaction mixture was stirred at 0° C. for 30 min. After quenching with water (5 ml), the mixture was extracted by CHCl3 (50 ml×2), washed with brine (50 ml×2). The organic layer was dried over Na2SO4 and concentrated in vacuo. The crude product was purified by column chromatography on silica gel (AcOEt/n-hexane=4/1) to afford the title compound 1 (648 mg, yield 54%). LC: 100%. MS: m/z=402.39, 403.18 (M+H+).

1. customAfter quenching with water (5 ml)
2. extractionthe mixture was extracted by CHCl3 (50 ml×2)
3. washwashed with brine (50 ml×2)
4. dry with materialThe organic layer was dried over Na2SO4
5. concentrationconcentrated in vacuo
6. customThe crude product was purified by column chromatography on silica gel (AcOEt/n-hexane=4/1)