反应详情

温度

105 °C

A mixture of [1-(4-azidopyridin-3-yl)meth-(E)-ylidene]-(2,6-dichlorophenyl)amine (7.2 mmol) in toluene (20 mL) was heated to 105° C. for 18 hours. The reaction mixture was cooled and concentrated under reduced pressure. The resultant residue was purified by silica gel flash chromatography (0-70% ethyl acetate in cyclohexane) to afford the title compound as a yellow solid (1.30 g, 68% yield). 1H NMR (300 MHz, CDCl3): δ 9.31 (d, J=1.4 Hz, 1H), 8.36 (d, J=6.4 Hz, 1H), 8.30 (d, J=1.0 Hz, 1H), 7.65 (dt, J=6.4, 1.2 Hz, 1H), 7.54-7.52 (m, 2H), 7.46 (dd, J=9.5, 6.4 Hz, 1H). LCMS (Method D): RT=3.46 min, m/z: 264 [M+H+].

1. temperatureThe reaction mixture was cooled
2. concentrationconcentrated under reduced pressure
3. customThe resultant residue was purified by silica gel flash chromatography (0-70% ethyl acetate in cyclohexane)