HRID617742

反应详情

EQUATION

反应方程式

HRID 617742 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Methyl 5-cyano-5-(2-fluorophenyl)-2-oxocyclohexane-1-carboxylate (D19, 30.66 g, 0.11 mol) was stirred at reflux in c. HCl (500 ml) for 17 h, cooled, diluted with water (500 ml), and extracted with ethyl acetate. This organic portion was extracted with potassium carbonate solution, dried (Na2SO4) and evaporated to give 4-cyano-4-(2-fluorophenyl)cyclohexanone (9.58 g, 38%) as a yellow foam. The alkaline extract was re-acidified with c. HCl, and the product isolated by extraction with ethyl acetate, drying (Na2SO4) and evaporation. This gave the title compound (16.36 g, 62%) as a colourless gum.

WORKUP

后处理

  1. temperatureat reflux in c
  2. temperaturecooled
  3. extractionextracted with ethyl acetate
  4. extractionThis organic portion was extracted with potassium carbonate solution
  5. dry with materialdried (Na2SO4)
  6. customevaporated