HRID261380

反应详情

EQUATION

反应方程式

HRID 261380 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 100 g (0.618 mole) of α,α,α-trifluoro-m-cresol, 106 g (0.632 mole) of ethyl bromoacetate, 87.5 g (0.632 mole) of potassium carbonate, and 1500 ml of acetone is stirred at reflux for 4 hours, and at room temperature for 18 hours. The mixture is filtered, evaporated under vacuum on a rotorary evaporator at 45° C. and at 85° C. (0.1 mm) to remove excess ethyl bromoacetate. The reaction mixture is taken up in 500 ml of ether, washed three times with 100 ml each of 0.1 M potassium carbonate, once with 100 ml of water, 100 ml of 0.01 M hydrochloric acid, and 100 ml of water. It is then dried with magnesium sulfate, filtered and evaporated, giving 142 g of the crude product. This is fractionally distilled at 73°-75° C. (0.1 mm) to give 124 g of the purified subject product as a colorless liquid.

WORKUP

后处理

  1. temperatureat reflux for 4 hours
  2. filtrationThe mixture is filtered
  3. customevaporated under vacuum on a rotorary evaporator at 45° C. and at 85° C. (0.1 mm)
  4. customto remove excess ethyl bromoacetate
  5. washwashed three times with 100 ml each of 0.1 M potassium carbonate
  6. dry with materialIt is then dried with magnesium sulfate
  7. filtrationfiltered
  8. customevaporated
  9. customgiving 142 g of the crude product
  10. distillationThis is fractionally distilled at 73°-75° C. (0.1 mm)