反应详情

A solution of [1-(4-azido-5-fluoropyridin-3-yl)meth-(E)-ylidene]-(2-chloro-6-fluorophenyl)amine (˜60 mmol) in toluene (250 mL) was heated under reflux for 3 hours. The resultant mixture was cooled to room temperature and concentrated under reduced pressure. The residue was triturated with diethyl ether and the solid obtained was collected by filtration and dried to afford the title compound as an off-white solid (9.96 g, 63% yield over two steps). 1H NMR (400 MHz, DMSO-d6): δ 9.32 (d, J=2.7 Hz, 1H), 9.20 (d, J=2.6 Hz, 1H), 8.29 (d, J=3.8 Hz, 1H), 7.81-7.74 (m, 1H), 7.72-7.60 (m, 2H).

1. temperatureunder reflux for 3 hours
2. concentrationconcentrated under reduced pressure
3. customThe residue was triturated with diethyl ether
4. customthe solid obtained
5. filtrationwas collected by filtration
6. customdried