反应详情

A solution of 2-{[1-(4-azido-5-fluoropyridin-3-yl)meth-(E)-ylidene]amino}-3-fluorobenzonitrile (5.19 g, 18.2 mmol) in toluene (90 mL) was heated under reflux for 4 hours. The resultant mixture was cooled to room temperature and concentrated under reduced pressure. The residue was purified by silica gel flash chromatography (50-100% ethyl acetate in cyclohexane) to afford the title compound as a beige solid (4.02 g, 86% yield). LCMS (Method C): RT=2.41 min, m/z: 257 [M+H+].

1. temperatureunder reflux for 4 hours
2. concentrationconcentrated under reduced pressure
3. customThe residue was purified by silica gel flash chromatography (50-100% ethyl acetate in cyclohexane)