反应详情

温度

20 °C

To a stirred solution of 4-vinylbenzene-1-sulfonyl chloride (950 mg, 4.69 mmol) in pyridine (8 mL) at 20° C. was added 5-chloro-2-fluoroaniline (682 mg, 4.69 mmol). The reaction mixture was stirred at 20° C. for 2 hours then evaporated in vacuo and redissolved in ethyl acetate. The organic phase was washed with saturated aqueous sodium carbonate (25 mL), dried using a hydrophobic frit and evaporated in vacuo to give the crude product as a yellow oil. The crude was purified by silica (Si) chromatography using a 0-25% ethyl acetate-cyclohexane gradient. The appropriate fractions were combined and evaporated in vacuo to give the required product, 822.7 mg as a white solid. LCMS [LCMS2] Rt 0.86 min, m/z (ES+) 312 (M+H).

1. customthen evaporated in vacuo
2. dissolutionredissolved in ethyl acetate
3. washThe organic phase was washed with saturated aqueous sodium carbonate (25 mL)
4. customdried
5. customevaporated in vacuo
6. customto give the crude product as a yellow oil
7. customThe crude was purified by silica (Si) chromatography
8. customevaporated in vacuo