HRID354967

反应详情

EQUATION

反应方程式

HRID 354967 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
140 °C

PROCEDURE

实验过程

A mixture of 21.5 parts of ethyl 4-hydroxy-1-piperidinecarboxylate, 35.2 parts of bis(4-fluorophenyl)bromomethane and 8.6 parts of potassium carbonate is stirred and heated in an oil-bath at 140° C. for 3 hours. The reaction mixture is allowed to cool to room temperature and water is added. The product is extracted with methylbenzene. The extract is washed successively with water, a diluted hydrochloric acid solution and a sodium bicarbonate solution, dried, filtered and evaporated. The forerun is distilled off (bp. till 143° C. at 0.5-1 mm. pressure), yielding ethyl 4-[bis(4-fluorophenyl)methoxy]-1-piperidinecarboxylate as an oily residue.

WORKUP

后处理

  1. temperatureto cool to room temperature
  2. extractionThe product is extracted with methylbenzene
  3. washThe extract is washed successively with water
  4. dry with materiala diluted hydrochloric acid solution and a sodium bicarbonate solution, dried
  5. filtrationfiltered
  6. customevaporated
  7. distillationThe forerun is distilled off (bp. till 143° C. at 0.5-1 mm. pressure)