反应详情

42 mg of 6-methoxy-1-oxo-4-(3-fluorophenyl)-1,2-dihydroisoquinoline-3-carbonitrile in 3 mL POCl3 was heated from room temp to 80 C. After 2 h, the temperature was raised to 90 C, and heating was continued for 20 h. The reaction was concentrated, redissolved in EtOAc, cooled to 0 C, and saturated aqueous sodium bicarbonate was added dropwise to quench the remaining reagent. The mixture was separated, and the aqueous solution was extracted with EtOAc (3×). The combined organic solutions were dried over MgSO4 and concentrated. Flash chromatography (3% to 30% EtOAc in hexanes) gave a white solid.

1. temperaturethe temperature was raised to 90 C
2. temperatureheating
3. waitwas continued for 20 h
4. concentrationThe reaction was concentrated
5. dissolutionredissolved in EtOAc
6. temperaturecooled to 0 C, and saturated aqueous sodium bicarbonate
7. additionwas added dropwise
8. customto quench the remaining reagent
9. customThe mixture was separated
10. extractionthe aqueous solution was extracted with EtOAc (3×)
11. dry with materialThe combined organic solutions were dried over MgSO4
12. concentrationconcentrated
13. customFlash chromatography (3% to 30% EtOAc in hexanes) gave a white solid