反应详情

温度

90 °C

7-Chloro-2-phenylquinazolin-4(3H)-one (3.11 g, 12.1 mmol) in POCl3 (40 mL) was heated with stirring at 90° C. under N2 for 2 d. The reaction was cooled to rt and evaporated to dryness under high vacuum. The residue was stirred for 30 min at 0° C. under Ar as a suspension in NH3/i-PrOH (2 M, 45 mL). Later DCM (˜100 mL) was added and stirring was continued for 1 h at rt. Aq NH4OH (conc, 50 mL) was added and layers were separated. The aqueous layer was extracted with DCM (2×). The organic phase was washed (satd NaHCO3, H2O, brine), dried (Na2SO4) and concentrated under reduced pressure to provide the title compound as a light yellow solid; 1H NMR (400 MHz, CD2Cl2) δ 8.56-8.46 (m, 2H), 8.14 (d, J=9.2 Hz, 1H), 8.02 (d, J=2.4 Hz, 1H), 7.56 (dd, J=2.4 Hz, 9.2 Hz, 1H), 7.52-7.45 (m, 3H).

1. temperatureThe reaction was cooled to rt
2. customevaporated to dryness under high vacuum
3. stirringThe residue was stirred for 30 min at 0° C. under Ar as a suspension in NH3/i-PrOH (2 M, 45 mL)
4. additionLater DCM (˜100 mL) was added
5. stirringstirring
6. waitwas continued for 1 h at rt
7. additionAq NH4OH (conc, 50 mL) was added
8. customlayers were separated
9. extractionThe aqueous layer was extracted with DCM (2×)
10. washThe organic phase was washed (satd NaHCO3, H2O, brine)
11. dry with materialdried (Na2SO4)
12. concentrationconcentrated under reduced pressure