HRID1447068

反应详情

EQUATION

反应方程式

HRID 1447068 的结构方程式

PROCEDURE

实验过程

A 100 g (0.48 mol) portion of phosphorus pentachloride is added to a flask containing 82.0 g (0.4 mol) of the above sulfonic acid salt. When the initial reaction subsides, the mixture is heated on the steam bath for 1 hr and 25 g of phosphorus pentachloride is added. Heating is continued for another 2.5 hr and another 10 g of phosphorus pentachloride is added and heating continued for 30 min. The dark reaction mixture is cooled and filtered and the filtrate distilled. The clear distillate is redistilled to give 42.3 g of 3-acetyloxy-1-propanesulfonyl chloride; bp 69°-81°/0.03 mm.

WORKUP

后处理

  1. customWhen the initial reaction subsides
  2. temperaturethe mixture is heated on the steam bath for 1 hr
  3. temperatureHeating
  4. temperatureheating
  5. waitcontinued for 30 min
  6. customThe dark reaction mixture
  7. temperatureis cooled
  8. filtrationfiltered
  9. distillationthe filtrate distilled
  10. distillationThe clear distillate is redistilled