HRID565614

反应详情

EQUATION

反应方程式

HRID 565614 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

500 ml of hexane and 70 ml of butyllithium (as a 2.5 molar solution in hexane) were introduced into a 1000 ml flask. 0.175 mol of 2-methylindene was added dropwise at the ambient temperature; the mixture was stirred for a further 10 hours. 0.18 mol of trimethylsilyl chloride was then added dropwise at room temperature; the mixture was stirred for a further 10 hours. LiCl was filtered off and 70 ml of butyllithium (as a 2.5 molar solution in hexane) were added to the clear filtrate. After further stirring for 10 hours, 0.18 mol of trimethylsilyl chloride was again added and the mixture was stirred for a further 10 hours. LiCl was filtered off and the solvent was removed in vacuo. Compound 54 remained as a colorless oil. Yield: 85% of the theoretical yield.

WORKUP

后处理

  1. stirringthe mixture was stirred for a further 10 hours
  2. filtrationLiCl was filtered off
  3. addition70 ml of butyllithium (as a 2.5 molar solution in hexane) were added to the clear filtrate
  4. stirringAfter further stirring for 10 hours
  5. stirringthe mixture was stirred for a further 10 hours
  6. filtrationLiCl was filtered off
  7. customthe solvent was removed in vacuo