HRID53022

反应详情

EQUATION

反应方程式

HRID 53022 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A suspension of 10.3 g of 4-benzoyl-2-butyl-5-cyano-1-tritylimidazole [prepared as described in step (i) above] in 80% v/v aqueous acetic acid was stirred at 60° C. for 5 hours. At the end of this time, the solution thus obtained was concentrated by evaporation under reduced pressure, and the concentrate was purified by column chromatography through silica gel, using a 2:1 by volume mixture of hexane and ethyl acetate as the eluent. The resulting oily product was dissolved in carbon tetrachloride and the solution was allowed to stand at room temperature, to precipitate crystals, which were collected by filtration to give 4.46 g of the title compound, melting at 121°-122° C.

WORKUP

后处理

  1. customAt the end of this time, the solution thus obtained
  2. concentrationwas concentrated by evaporation under reduced pressure
  3. customthe concentrate was purified by column chromatography through silica gel
  4. additionby volume mixture of hexane and ethyl acetate as the eluent
  5. dissolutionThe resulting oily product was dissolved in carbon tetrachloride
  6. customto stand at room temperature
  7. customto precipitate crystals, which
  8. filtrationwere collected by filtration