反应详情

A mixture of 3-amino-4-(4'-cyanophenyl)aminopyridine (420 mg, 2.0 mmol) (prepared as above), trifluoroacetaldehyde hydrate (232 mg, 2.0 mmol), and sodium metabisulphite (475 mg, 2.5 mmol) in N,N-dimethylacetamide (10 ml) was heated under reflux for 16 hours. After being cooled, the mixture was diluted with ethyl acetate (200 ml), washed with saturated aqueous sodium bicarbonate (50 ml) and water (5×50 ml). The organic layer was dried (MgSO4) and concentrated under reduced pressure. The residue was purified by flash chromatography (eluting with ethyl acetate) to give 1-(4-cyanophenyl)-2-trifluoromethylimidazo[4,5-c]pyridine, 337 mg.

1. temperaturewas heated
2. temperatureunder reflux for 16 hours
3. temperatureAfter being cooled
4. washwashed with saturated aqueous sodium bicarbonate (50 ml) and water (5×50 ml)
5. dry with materialThe organic layer was dried (MgSO4)
6. concentrationconcentrated under reduced pressure
7. customThe residue was purified by flash chromatography (eluting with ethyl acetate)