反应详情

7-Bromo[1]benzothieno[2,3-d]pyrimidin-4(3H)-one (7.80 g, 27.7 mmol), POCl3 (70 mL) and triethylamine (70 mL) were heated in an oil bath at 80° C. for 3 h. The resulting slurry was concentrated on a rotavap, slurried in dichloromethane and poured into 500 mL of satd NaHCO3. The organic phase was then washed with satd NaHCO3, water, and then collected. The initial aqueous phase (pH<1) was basified with 1.0 N NaOH and extracted with dichloromethane. The organic layers were combined, dried with sodium sulfate, filtered, and concentrated under high vacuum to yield a crude brown solid (7.6 g, 91%). 1H NMR (DMSO-d6) δ 9.05 (s, 1H), 8.60 (d, 1H), 8.60 (s, 1H), 7.88 (d, 1H).

1. concentrationThe resulting slurry was concentrated on a rotavap
2. additionpoured into 500 mL of satd NaHCO3
3. washThe organic phase was then washed with satd NaHCO3, water
4. customcollected
5. extractionextracted with dichloromethane
6. dry with materialdried with sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated under high vacuum