反应详情

Thionyl chloride (8.1 mL, 111.19 mmol) was added dropwise at 0° C. to a solution of 2-(4-chloro-2-methoxy-phenyl)-ethenesulfonic acid (5.53 g, 22.24 mmol) in DMF (10 mL). The reaction mixture was stirred at RT for 3 h and then was poured onto crushed ice. Ethyl acetate (50 mL) was added to the mixture. The organic phase was separated, washed with brine (3×20 mL), dried over MgSO4 and concentrated under reduced pressure. The oily residue was purified on silica gel using hexane/ethyl acetate, 4:1 to give the target compound which was then recrystallized from pentane/diethyl ether to afford the title compound (2.30 g, 61% over 3 steps) as a white solid.

1. additionwas poured
2. customonto crushed ice
3. customThe organic phase was separated
4. washwashed with brine (3×20 mL)
5. dry with materialdried over MgSO4
6. concentrationconcentrated under reduced pressure
7. customThe oily residue was purified on silica gel
8. customto give the target compound which
9. customwas then recrystallized from pentane/diethyl ether