HRID35477

反应详情

EQUATION

反应方程式

HRID 35477 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

53.5 g of 2-[[(4-methoxy-3,5-dimethyl-2 -pyridyl)methyl]thio]benzimidazole are dissolved in 1.2 l of methylene chloride and 100 ml of methanol and then cooled to -20°. 33.4 g of m-chloroperbenzoic acid, recrystallized from methylene chloride/petroleum ether, are then introduced within 10 minutes. The solution is stirred for a further 60 minutes at -20° and then poured into a mixture of 250 ml of 2N sodium carbonate solution and ice. The organic phase is washed neutral with water, dried over sodium sulphate and evaporated in vacuo. Crystallization from methylene chloride/methanol/petroleum ether gives 2-[[(4-methoxy-3,5-dimethyl-2-pyridyl)methyl]sulphinyl]benzimidazole of melting point 157°-159°.

WORKUP

后处理

  1. custom33.4 g of m-chloroperbenzoic acid, recrystallized from methylene chloride/petroleum ether
  2. additionare then introduced within 10 minutes
  3. additionpoured into a mixture of 250 ml of 2N sodium carbonate solution and ice
  4. washThe organic phase is washed neutral with water
  5. dry with materialdried over sodium sulphate
  6. customevaporated in vacuo
  7. customCrystallization from methylene chloride/methanol/petroleum ether