反应详情

A mixture of 2-[N-butyryl-N-[4-(4-chloro-2-cyano-1-pyrrolyl)benzyl]amino]-4-methyl-3-nitropyridine (700 mg), iron powder (894 mg), acetic acid (1.8 ml) and ethanol (15 ml) was stirred under reflux for 15 hours. After being cooled to room temperature, the reaction mixture was filtered and the filtrate was evaporated in vacuo. The residue was partitioned into ethyl acetate (100 ml) and saturated aqueous sodium hydrogencarbonate solution. The organic layer was washed with water, dried over magnesium sulfate and evaporated in vacuo. The residue was purified by a silica gel column chromatography (n-hexane-ethyl acetate =1:1) to give 3-[4-(4-chloro-2-cyano-1-pyrrolyl)benzyl]-7-methyl-2-propyl-3H-imidazo[4,5-b]pyridine (565 mg) as a pale yellow powder.

1. temperatureunder reflux for 15 hours
2. filtrationthe reaction mixture was filtered
3. customthe filtrate was evaporated in vacuo
4. customThe residue was partitioned into ethyl acetate (100 ml) and saturated aqueous sodium hydrogencarbonate solution
5. washThe organic layer was washed with water
6. dry with materialdried over magnesium sulfate
7. customevaporated in vacuo
8. customThe residue was purified by a silica gel column chromatography (n-hexane-ethyl acetate =1:1)