反应详情

温度

55 °C

5-Carbamoyl-2-methoxybenzenesulfonyl chloride (150 g) was suspended in 1800 mL of ethyl acetate. After 219 mL of thionyl chloride was dropped to the stirred suspension under ice-cooling, 2.3 mL of N,N-dimethylformamide was added to the mixture. After being stirred at 55° C. for 3 hours, the reaction mixture was concentrated under reduced pressure. To the residue were added ethyl acetate and water, and the separated organic layer was washed with water, saturated aqueous sodium bicarbonate solution, and brine, and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure, and the obtained crude product was recrystallized from ethyl acetate-hexane to give 86.8 g of 5-cyano-2-methoxybenzenesulfonyl chloride.

1. temperaturecooling
2. concentrationthe reaction mixture was concentrated under reduced pressure
3. additionTo the residue were added ethyl acetate and water
4. washthe separated organic layer was washed with water, saturated aqueous sodium bicarbonate solution, and brine
5. dry with materialdried over anhydrous magnesium sulfate
6. customThe solvent was removed under reduced pressure
7. customthe obtained crude product
8. customwas recrystallized from ethyl acetate-hexane