HRID1859394

反应详情

EQUATION

反应方程式

HRID 1859394 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a mixture of ethyl trifluoroacetate (17.2 g) and sodium hydride (60% in oil, 5.7 g) in THF (200 ml) is added a solution of 1A (11.2 g) in THF (50 ml) with ethanol (2 drops) and a solution of dibenzo-18-crown-6 (415 mg) in THF (70 ml). The reaction mixture is stirred for 60 h at ambient temperature. After heating for 1 h at reflux temperature, the mixture is acidified with 2M hydrochloric acid and extracted with ethyl acetate. The organic phase is dried and evaporated. One obtains the crude title compound as an oily product (21.5 g).

WORKUP

后处理

  1. temperatureAfter heating for 1 h
  2. temperatureat reflux temperature
  3. extractionextracted with ethyl acetate
  4. customThe organic phase is dried
  5. customevaporated