HRID13853

反应详情

EQUATION

反应方程式

HRID 13853 的结构方程式

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

A 100 mL Hastelloy shaker tube was loaded with 26.5 g (0.227 mole) chlorosulfuric acid, cooled in liquid nitrogen, evacuated and loaded with 30 g (0.225 mole) of 1,1,3,3,3-pentafluoropropene. The reaction vessel was allowed to warm and kept on a shaker at 40° C. at autogenous pressure for 6 hours. The pressure tube was unloaded, and the reaction mixture was added drop by drop into the flask containing 60 ml of ethanol at −10° C. over a 15 minute period. The reaction mixture was stirred overnight at 20° C. and then was poured into 200 ml of ice water. The organic layer was separated, washed with sodium bicarbonate, water, and dried under MgSO4. Distillation gave 31 g of CF3CH2COOEt (87%), bp 108-109° C.

WORKUP

后处理

  1. temperaturecooled in liquid nitrogen
  2. customevacuated
  3. temperatureto warm
  4. additionthe reaction mixture was added drop by drop into the flask
  5. customThe organic layer was separated
  6. washwashed with sodium bicarbonate, water
  7. customdried under MgSO4
  8. distillationDistillation