HRID580663

反应详情

EQUATION

反应方程式

HRID 580663 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-20 °C

PROCEDURE

实验过程

10 Parts of 3-cyclopentyl propionic acid are dissolved in 150 parts by volume of ethyl ether and chilled to -20° C. under argon. 50 Parts by volume of 2.8 molar methyl magnesium bromide are added dropwise. After the addition of the methyl magnesium bromide is completed, the mixture is allowed to warm to room temperature. The cloudy reaction mixture is treated with 1N hydrochloric acid and the clearified reaction mixture is extracted with ether followed by ethyl acetate. The combined organic extracts are washed with water and saturated sodium chloride solution, dried over anhydrous sodium sulfate, filtered and the solvent evaporated under reduced pressure. The residual oil is chromatographed on silica gel using 10% ethyl acetate/hexane as the eluent, to provide 4-cyclopentyl-2-butanone.

WORKUP

后处理

  1. temperatureto warm to room temperature
  2. customThe cloudy reaction mixture
  3. extractionthe clearified reaction mixture is extracted with ether
  4. washThe combined organic extracts are washed with water and saturated sodium chloride solution
  5. dry with materialdried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. customthe solvent evaporated under reduced pressure
  8. customThe residual oil is chromatographed on silica gel using 10% ethyl acetate/hexane as the eluent