HRID56617
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
A solution of 1.9 g (8.1 mmol) of ethyl 6-nitro-1H-benzimidazole-2-carboxylate in 30 ml of ethanol was hydrogenated in the presence of 190 mg of palladium (10% on activated carbon) at RT and standard pressure for 3 h. The reaction mixture was then filtered through kieselguhr and the residue was washed with ethanol. The combined filtrates were concentrated under reduced pressure. The residue was dried under reduced pressure and then purified by flash chromatography (silica gel 50, mobile phase: dichloromethane/methanol 3-5%). Yield: 640 mg (39% of theory)
WORKUP
后处理
- filtrationThe reaction mixture was then filtered through kieselguhr
- washthe residue was washed with ethanol
- concentrationThe combined filtrates were concentrated under reduced pressure
- customThe residue was dried under reduced pressure
- custompurified by flash chromatography (silica gel 50, mobile phase: dichloromethane/methanol 3-5%)