HRID271016

反应详情

EQUATION

反应方程式

HRID 271016 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of 2.5 g (17.6 mmol) of phenylcyclopentadiene in 30 ml of toluene was ice cooled, and thereto was dropwise added 13.0 ml (21.1 mmol) of a hexane solution of n-butyllithium. The resulting white slurry was stirred at room temperature for one night. From the slurry, the solvent was filtered off to give a THF solution (brown solution). To the solution, a solution of 3.2 g (17.6 mmol) of benzophenone in 10 ml of THF was added, followed by stirring at room temperature for one night. After addition of water, the mixture was subjected to extraction with diethyl ether and dried over magnesium sulfate. Then, the ether was distilled off to obtain a red viscous liquid. The liquid was purified by a silica gel column to obtain a red solid.

WORKUP

后处理

  1. temperaturecooled
  2. filtrationFrom the slurry, the solvent was filtered off
  3. customto give a THF solution (brown solution)
  4. stirringby stirring at room temperature for one night
  5. extractionthe mixture was subjected to extraction with diethyl ether
  6. dry with materialdried over magnesium sulfate
  7. distillationThen, the ether was distilled off
  8. customto obtain a red viscous liquid
  9. customThe liquid was purified by a silica gel column
  10. customto obtain a red solid