HRID1979538

反应详情

EQUATION

反应方程式

HRID 1979538 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In 200 ml. of benzene was dissolved 50 g. of farnesyl acetone, and then 28 g. of ethyl cyanoacetate, 5 g. of ammonium acetate and 5 g. of acetic acid were added to the solution. The mixture was then refluxed for 8 hours with removal of the produced water. The reaction mixture then was washed with water and dried. To this mixture there was added dropwise a solution of 4.3 g. of sodium borohydride in 50 ml. of ethanol, under stirring and at 10°-20° C. The stirring was continued for 1 hour. Then, 50 ml. of 10% acetic acid was added to the reaction mixture, and the mixture was subsequently washed with water and dried. The solvent was removed by evaporation and then the residue was purified by silica gel column chromatography to obtain 50.5 g. of the desired oily product.

WORKUP

后处理

  1. washThe reaction mixture then was washed with water
  2. customdried
  3. additionTo this mixture there was added dropwise a solution of 4.3 g
  4. additionof 10% acetic acid was added to the reaction mixture
  5. washthe mixture was subsequently washed with water
  6. customdried
  7. customThe solvent was removed by evaporation
  8. customthe residue was purified by silica gel column chromatography
  9. customto obtain 50.5 g