HRID381446

反应详情

EQUATION

反应方程式

HRID 381446 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

In 4 ml of toluene were dissolved 480 mg (1.79 mmol) of ethyl (E)-5-[4-(trifluoromethyl)phenyl]-2-penten-4-ynoate, and 2.38 ml (3.58 mmol) of a 1.5 M diisobutyl aluminum hydride-toluene solution were added to the solution with stirring at 0° C. After 10 minutes, ice was added to the mixture and the insolubles were removed by filtration using Celite. After the organic layer was dried, the crude product obtained by evaporation of the solvent was subjected to column chromatography using 15 g of silica gel and eluted with a mixed solvent of ethyl acetate-hexane (3:17) to obtain 353 mg (yield: 87%) of the title compound as an oil.

WORKUP

后处理

  1. additionwere added to the solution
  2. additionice was added to the mixture
  3. customthe insolubles were removed by filtration
  4. customAfter the organic layer was dried
  5. customthe crude product obtained by evaporation of the solvent
  6. washeluted with a mixed solvent of ethyl acetate-hexane (3:17)