HRID1769582

反应详情

EQUATION

反应方程式

HRID 1769582 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of triethyl phosphonoacetate (21.8 g) in THF (50 ml) was stirred in a nitrogen gas stream, followed by adding potassium-t-butoxide (11.8 g) little by little at room temperature, stirring the reaction solution at room temperature for one hour, dropwise adding a solution of 4-(3',4',5'-trifluorophenyl)cyclohexanone (20 g) in THF (50 ml), stirring at room temperature for 2 hours, adding to water (100 ml), extracting with ethyl acetate (100 ml), washing the organic layer with water, drying over anhydrous MgSO4 and concentrating the solvent under reduced pressure, to obtain 4-(3',4',5'-trifluorophenyl))ethoxycarbonylmethylenecyclohexane (18.3 g).

WORKUP

后处理

  1. stirringstirring the reaction solution at room temperature for one hour
  2. stirringstirring at room temperature for 2 hours
  3. extractionextracting with ethyl acetate (100 ml)
  4. washwashing the organic layer with water
  5. dry with materialdrying over anhydrous MgSO4
  6. concentrationconcentrating the solvent under reduced pressure