HRID333954

反应详情

EQUATION

反应方程式

HRID 333954 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Ethyl (E)-4,4,5,5,5-pentafluoropent-2-enoate (5.5 g, 25.2 mmol) was suspended in 10% NaOH (14.5 ml) and heated at reflux until a homogenous solution was obtained (40 min). After cooling the mixture was washed with diethylether (2×) and acidified under ice-cooling with concentrated sulfuric acid. The mixture was extracted with diethylether (3×), the combined organic phases were washed with water, dried over magnesium sulfate and the solvent removed under reduced pressure. 2.64 g (13.9 mmol, 55%) were obtained. MS (ES) M/z=189.0 [M−H]−.

WORKUP

后处理

  1. temperatureheated
  2. temperatureat reflux until a homogenous solution
  3. customwas obtained (40 min)
  4. temperatureAfter cooling the mixture
  5. washwas washed with diethylether (2×)
  6. temperaturecooling with concentrated sulfuric acid
  7. extractionThe mixture was extracted with diethylether (3×)
  8. washthe combined organic phases were washed with water
  9. dry with materialdried over magnesium sulfate
  10. customthe solvent removed under reduced pressure
  11. custom2.64 g (13.9 mmol, 55%) were obtained