HRID53022
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customAt the end of this time, the solution thus obtained
- concentrationwas concentrated by evaporation under reduced pressure
- customthe concentrate was purified by column chromatography through silica gel
- additionby volume mixture of hexane and ethyl acetate as the eluent
- dissolutionThe resulting oily product was dissolved in carbon tetrachloride
- customto stand at room temperature
- customto precipitate crystals, which
- filtrationwere collected by filtration