反应详情

A suspension of 4-{[1-(4-azido-5-chloropyridin-3-yl)meth-(E)-ylidene]amino}-3,5-dichlorobenzonitrile (3.8 g, 10.95 mmol) in toluene (45 mL) was heated to reflux for 18 hours and then cooled to room temperature. The precipitated solid was removed by filtration and washed sequentially with toluene, ethyl acetate and DCM. The filtrate was concentrated under reduced pressure. The residue was purified by silica gel flash chromatography (0-100% ethyl acetate in cyclohexane) and then triturated with diethyl ether to afford the title compound as an off-white solid (2.5 g, 71% yield). 1H NMR (400 MHz, CDCl3): δ 9.30 (s, 1H), 8.46 (s, 1H), 8.42 (s, 1H), 7.86 (s, 2H).

1. temperaturewas heated
2. temperatureto reflux for 18 hours
3. customThe precipitated solid was removed by filtration
4. washwashed sequentially with toluene, ethyl acetate and DCM
5. concentrationThe filtrate was concentrated under reduced pressure
6. customThe residue was purified by silica gel flash chromatography (0-100% ethyl acetate in cyclohexane)
7. customtriturated with diethyl ether