反应详情

温度

60 °C

Under an argon atmosphere, metal sodium (635 mg) was added to anhydrous ethanediol (12 mL), and the mixture was stirred at 60° C. for 3 hr. Then, 2-chloro-1-methyl-1H-benzimidazole (4.0 g) was added and the mixture was stirred with heating at 90° C. for 5 hr. The mixture was allowed to cool to room temperature, diluted with water and extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (3.0 g).

1. stirringthe mixture was stirred
2. temperaturewith heating at 90° C. for 5 hr
3. temperatureto cool to room temperature
4. extractionextracted with ethyl acetate
5. washThe organic layer was washed with saturated brine
6. dry with materialdried over magnesium sulfate
7. concentrationconcentrated under reduced pressure
8. customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane)