反应详情

To a suspension of 2-(2,6-dichloro-4-iodophenyl)-7-fluorothiazolo[5,4-c]pyridine-5-oxide (2.8 g, 6.4 mmol) in 1,2-dichloroethane (80 mL) was added phosphorus oxychloride (1.8 mL, 19.1 mmol). The reaction mixture was heated under reflux for 16 hours. Upon cooling, the resultant mixture was treated cautiously with aqueous sodium bicarbonate to achieve pH 6-7, and then extracted with dichloromethane (×2). The combined organic extracts were dried (MgSO4), filtered and concentrated under reduced pressure. The crude product was purified by column chromatography on silica gel eluting with 0-50% diethyl ether in petroleum ether to afford the title compound as a white solid (1.0 g, 34% yield). 1H NMR (400 MHz, CDCl3): δ 8.35 (d, J=1.5 Hz, 1H), 7.82 (s, 2H).

1. temperatureThe reaction mixture was heated
2. temperatureunder reflux for 16 hours
3. temperatureUpon cooling
4. extractionextracted with dichloromethane (×2)
5. dry with materialThe combined organic extracts were dried (MgSO4)
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure
8. customThe crude product was purified by column chromatography on silica gel eluting with 0-50% diethyl ether in petroleum ether