反应详情

A mixture of 2-chloro-N-(2-chloro-3-fluoro-pyridine-4-yl)-6-fluorobenzamide (600 mg, 2 mmol) and thionyl chloride (5 mL) was heated under reflux for 16 hours then cooled to ambient temperature. The reaction mixture was diluted with toluene (6 mL) and concentrated to dryness under reduced pressure to give the desired compound as a brown oil (650 mg, quant. yield). 1H NMR (400 MHz, CDCl3): δ 8.23 (d, J=5.1 Hz, 1H), 7.44 (td, J=8.3, 5.6 Hz, 1H), 7.33 (d, J=8.2 Hz, 1H), 7.16 (t, J=8.7 Hz, 1H), 6.97 (t, J=5.1 Hz, 1H).

1. temperaturewas heated
2. temperatureunder reflux for 16 hours
3. concentrationconcentrated to dryness under reduced pressure