反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- custom33.4 g of m-chloroperbenzoic acid, recrystallized from methylene chloride/petroleum ether
- additionare then introduced within 10 minutes
- additionpoured into a mixture of 250 ml of 2N sodium carbonate solution and ice
- washThe organic phase is washed neutral with water
- dry with materialdried over sodium sulphate
- customevaporated in vacuo
- customCrystallization from methylene chloride/methanol/petroleum ether