反应详情

温度

50 °C

A 96.8-g (0.632 mol) sample of 2,5-dichlorothiophene was added dropwise to a cooled (dry ice/acetone bath, about -10° to -15° C.) and stirred solution of 163 g (1.39 mol) of chlorosulfonic acid. After the addition was completed, the reaction mixture was stirred at 50° C for 2 hours, cooled, and then poured into 200 g of ice. The aqueous reaction mixture was extracted with methylene chloride. The methylene chloride extract was washed with saturated aqueous sodium bicarbonate solution, washed with water, dried over magnesium sulfate, and evaporated to give 87 g of 2,5-dichloro-3-thienylsulfonyl chloride.

1. additionAfter the addition
2. temperaturecooled
3. extractionThe aqueous reaction mixture was extracted with methylene chloride
4. extractionThe methylene chloride extract
5. washwas washed with saturated aqueous sodium bicarbonate solution
6. washwashed with water
7. dry with materialdried over magnesium sulfate
8. customevaporated