HRID1709767

反应详情

EQUATION

反应方程式

HRID 1709767 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of 13.7 g of 5,6-difluoro-2-[[(4-methoxy 3-methyl-2-pyridyl)methyl]thio]benzimidazole in 800 ml of methylene chloride and 130 ml of methanol was treated with 6.9 g of potassium carbonate. 9.6 g of m-chloroperbenzoic acid were added thereto at -30°, whereupon the solution was stirred for a further 5 minutes and subsequently poured into a mixture of 200 ml of saturated sodium bicarbonate solution and 200 ml of water. The separated organic phase was dried over sodium sulfate, treated with 5.0 ml of triethylamine and evaporated in a vacuum. Crystallization from methylene chloride-methanol-ether yielded 5,6-difluoro-2-[[(4-methoxy-3-methyl-2-pyridyl))methyl]sulfinyl]benzimidazole of melting point 188°-189°.

WORKUP

后处理

  1. dry with materialThe separated organic phase was dried over sodium sulfate
  2. additiontreated with 5.0 ml of triethylamine
  3. customevaporated in a vacuum
  4. customCrystallization from methylene chloride-methanol-ether