HRID2165937

反应详情

EQUATION

反应方程式

HRID 2165937 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a mixture of 2-[3-(4-acetyl-3-hydroxy-2-propylphenoxy)-propylthio]benzimidazole-5-carboxylic acid (1.00 g) in dichloromethane (30 ml) and methanol (3 ml) stirring in ice-salt-water bath, was added m-chloroperbenzoic acid (80%, 503 mg) in a small portions below 0° C. Further stirring for an additional 15 minutes, the mixture was evaporated, and the residue was purified by silica gel chromatography, eluting with dichloromethane-ethyl acetate-methanol (10:2:1), and recrystallized from ethanol-water to give the title compound (540 mg, 52.1%) as colorless crystals, mp 173-175° C.

WORKUP

后处理

  1. customthe mixture was evaporated
  2. customthe residue was purified by silica gel chromatography
  3. washeluting with dichloromethane-ethyl acetate-methanol (10:2:1)
  4. customrecrystallized from ethanol-water