HRID1647153
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
5-Acetyl-6-methyl-2-[[(3,4-methylenedioxy-2pyridinyl)methyl]thio]-1H-benzimidazole (140 mg, 0,41 mmol) was dissolved in methylene chloride (20 ml) and sodium hydrogen carbonate (5 ml,1M). The mixture was stirred at ambient temperature and MCPBA (100 mg, 0.41 mmol, 70%) dissolved in methylene chloride (10 ml) was added portionwise. After 10 min sodium thiosulphate (100 mg) was added whereupon the phases were separated. The organic phase was dried over sodium sulphate, filtered and concentrated under reduced pressure. The residue was chromatographed on silica (CH2Cl2 /MeOH/NH3, 97.5: 2.5: sat.) Yield: 90 mg (61%) of the title compound. Mp: 178°-180° C. (dec., uncorr.).
WORKUP
后处理
- additionwas added portionwise
- customwere separated
- dry with materialThe organic phase was dried over sodium sulphate
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customThe residue was chromatographed on silica (CH2Cl2 /MeOH/NH3, 97.5: 2.5: sat.) Yield: 90 mg (61%) of the title compound