HRID265162

反应详情

EQUATION

反应方程式

HRID 265162 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

A mixture of 1.3 g of 2-butyl-5-cyano-4-(1-hydroxy-1-methylethyl)-1-tritylimidazole [prepared as described in step (i) above] and 26 ml of 75% v/v aqueous acetic acid was stirred at 50° C. for 3 hours, and then the solvent was removed by distillation under reduced pressure. The resulting residue was washed with carbon tetrachloride and purified by column chromatography through silica gel, using a 10:1 by volume mixture of methylene chloride and methanol as the eluent, and the product was crystallized in carbon tetrachloride, to give 0.6 g of the title compound as colorless crystals, melting at 171°-172° C.

WORKUP

后处理

  1. customthe solvent was removed by distillation under reduced pressure
  2. washThe resulting residue was washed with carbon tetrachloride
  3. custompurified by column chromatography through silica gel
  4. additionby volume mixture of methylene chloride and methanol as the eluent
  5. customthe product was crystallized in carbon tetrachloride