反应详情

522 g of 2-n-butylbenzimidazole was dissolved in 10 ml of dimethylformamide and dropwise added to 130 g of sodium hydride. The mixture was stirred at room temperature for 30 min, and 920 mg of 2-(4-bromomethylphenyl)-4-chlorobenzonitrile dissolved in 10 ml of dimethylformamide was dropwise added thereto. The mixture was stirred at room temperature for 10 min, and the reaction mixture was filtered. The filtrate was concentrated and water and ethyl acetate were added to the residue. The organic phase was separated, dried over anhydrous magnesium sulfate and then concentrated. The residue was purified by column chromatography (chloroform:ethanol=98:2) (yield: 1.12 g).

1. additionwas dropwise added
2. stirringThe mixture was stirred at room temperature for 10 min
3. filtrationthe reaction mixture was filtered
4. concentrationThe filtrate was concentrated
5. additionwater and ethyl acetate were added to the residue
6. customThe organic phase was separated
7. dry with materialdried over anhydrous magnesium sulfate
8. concentrationconcentrated
9. customThe residue was purified by column chromatography (chloroform:ethanol=98:2) (yield: 1.12 g)