HRID52906

反应详情

EQUATION

反应方程式

HRID 52906 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 0.28 g of ethyl 4-hydroxymethyl-2-propyl-{4-[2-(trityltetrazol-5-yl)phenyl]phenyl}methylimidazole-5-carboxylate [prepared as described in step (b) above] in 4 ml of 75% v/v aqueous acetic acid was stirred at 60° C. for 2 hours. The reaction mixture was then concentrated by evaporation under reduced pressure, and the residue was dissolved in toluene. The resulting solution was again concentrated by evaporation under reduced pressure, to remove as much water and acetic acid as possible. The residue was then purified by column chromatography through silica gel, using 9:1 and 4:1 by volume mixtures of methylene chloride and methanol as the eluent, to give 0.20 g of the title compound as an amorphous solid.

WORKUP

后处理

  1. concentrationThe reaction mixture was then concentrated by evaporation under reduced pressure
  2. dissolutionthe residue was dissolved in toluene
  3. concentrationThe resulting solution was again concentrated by evaporation under reduced pressure
  4. customto remove as much water and acetic acid as possible
  5. customThe residue was then purified by column chromatography through silica gel