反应详情

An aqueous solution (20 ml) of (2-(4-nitrophenyl)-1-(1-propylimidazol-2-yl)ethanone (1.2 g), reduced iron (1.2 g) and anhydrous calcium chloride (244 mg) in 85% ethanol was stirred for 4 hours under nitrogen atmosphere at 105° C. The mixture was allowed to be at room temperature, ethyl acetate was added to the mixture, the insolubles were filtered off, and water was added to separate the layers. The organic layer was washed with saturated brine, and dried over magnesium sulfate. The solvent was distilled off under reduced pressure and the obtained residue was purified by silica gel column chromatography (hexane:ethyl acetate=0.4:1) to give 2-(4-aminophenyl)-1-(1-propylimidazol-2-yl)ethanone (863 mg) as red oil.

1. customto be at room temperature
2. filtrationthe insolubles were filtered off
3. additionwater was added
4. customto separate the layers
5. washThe organic layer was washed with saturated brine
6. dry with materialdried over magnesium sulfate
7. distillationThe solvent was distilled off under reduced pressure
8. customthe obtained residue was purified by silica gel column chromatography (hexane:ethyl acetate=0.4:1)