HRID2165769

反应详情

EQUATION

反应方程式

HRID 2165769 的结构方程式

PROCEDURE

实验过程

12.8 parts of 1-(4-chloro-2-difluoromethoxyphenyl)ethan-1-one and 10.4 parts of 1,2-butanediol are heated under reflux for 12 hours in 100 ml of abs. toluene in the presence of 0.2 part of p-toluenesulfonic acid as catalyst, while removing the water of reaction with a water separator. The reaction mixture is cooled to room temperature and then washed with 2×100 ml of water, dried over sodium sulfate and filtered. The solvent is removed by evaporation and the residual oil is purified by high-vacuum distillation; b.p. 78°-80° C./0.04 mbar.

WORKUP

后处理

  1. temperatureunder reflux for 12 hours in 100 ml of abs
  2. customtoluene in the presence of 0.2 part of p-toluenesulfonic acid as catalyst, while removing
  3. customthe water of reaction with a water separator
  4. washwashed with 2×100 ml of water
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. customThe solvent is removed by evaporation
  8. distillationthe residual oil is purified by high-vacuum distillation