HRID1709759

反应详情

EQUATION

反应方程式

HRID 1709759 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2.0 g of 5-fluoro-2-[[(4-methoxy-3-methyl-2-pyridyl)methyl]thio]benzimidazole dissolved in 100 ml of methylene chloride were treated with 1.2 g of potassium carbonate. 1.6 g of m-chloroperbenzoic acid were added thereto at -30°, the solution was stirred for a further 5 minutes and subsequently poured into a mixture of 30 ml of saturated sodium bicarbonate solution and 30 ml of water. The organic phase was separated, dried over sodium sulfate, treated with 5.0 ml of triethylamine and evaporated in a vacuum. Crystallization of the residue from methylene chloride/petroleum ether (low boiling)/ether gave 5-fluoro-2-[[(4-methoxy-3-methyl-2-pyridyl)methyl]sulfinyl]benzimidazole of melting point 175°.

WORKUP

后处理

  1. customThe organic phase was separated
  2. dry with materialdried over sodium sulfate
  3. additiontreated with 5.0 ml of triethylamine
  4. customevaporated in a vacuum
  5. customCrystallization of the residue from methylene chloride/petroleum ether (low boiling)/ether