HRID56617

反应详情

EQUATION

反应方程式

HRID 56617 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. filtrationThe reaction mixture was then filtered through kieselguhr
  2. washthe residue was washed with ethanol
  3. concentrationThe combined filtrates were concentrated under reduced pressure
  4. customThe residue was dried under reduced pressure
  5. custompurified by flash chromatography (silica gel 50, mobile phase: dichloromethane/methanol 3-5%)