反应详情

温度

105 °C

A mixture of 4-{[1-(4-azidopyridin-3-yl)meth-(E)-ylidene]amino}-3,5-dichlorobenzonitrile (21.4 mmol) in toluene (80 mL) was heated to 105° C. for 1 hour. The reaction mixture was cooled and concentrated under reduced pressure. The resultant residue was purified by silica gel flash chromatography (0-100% ethyl acetate in cyclohexane) to afford the title compound as a yellow solid (4.10 g, 66% yield). 1H NMR (300 MHz, CDCl3): δ 9.36 (d, J=1.4 Hz, 1H), 8.39 (d, J=6.5 Hz, 1H), 8.35 (d, J=1.0 Hz, 1H), 7.85 (s, 2H), 7.68-7.66 (m, 1H). LCMS (Method D): RT=1.66 min, m/z: 289 [M+H+].

1. temperatureThe reaction mixture was cooled
2. concentrationconcentrated under reduced pressure
3. customThe resultant residue was purified by silica gel flash chromatography (0-100% ethyl acetate in cyclohexane)