HRID325594

反应详情

EQUATION

反应方程式

HRID 325594 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
95 °C

PROCEDURE

实验过程

33.4 g of 2-(2-fluorobenzyloxy)ethyl-2-(4-hydroxyphenoxy)propionate was dissolved in 120 ml of dimethylformamide, 15.2 g of potassium carbonate were added thereto, then the mixture was heated at 95° C. for one hour with stirring. 27.1 g of 4-trifluoromethyl chlorobenzene were added to the solution which was then heated to 95° to 100° C. for five hours. After cooling the reaction solution to room temperature, it was poured into ice-water, then extracted with toluene. The toluene layer was washed successively with 1% strength by weight sodium hydroxide solution and water, and was dried and filtered. The toluene was distilled off under reduced pressure, and further volatile by-products were removed at 100° C./0.1 mmHg. The end product of 2-(2-fluorobenzyloxy)ethyl-2-[4-(4-trifluoromethylphenoxy)phenoxy]propionate was obtained in a yield of 20.7 g. (nD20 1.5235)

WORKUP

后处理

  1. temperaturewas then heated to 95° to 100° C. for five hours
  2. temperatureAfter cooling the reaction solution to room temperature
  3. extractionextracted with toluene
  4. washThe toluene layer was washed successively with 1% strength by weight sodium hydroxide solution and water
  5. customwas dried
  6. filtrationfiltered
  7. distillationThe toluene was distilled off under reduced pressure, and further volatile by-products
  8. customwere removed at 100° C./0.1 mmHg