反应详情

温度

65 °C

N, N-dimethylaniline (0.37 ml, 1.23 mmol) was added dropwise to a solution of 8-nitro-3H-quinazolin-4-one 476 (200 mg, 1.04 mmol) in POCl3 (1.25 ml, 10.5 mmol) at 0° C. The mixture was heated at 65° C. for 1.5 h. After cooling, the mixture was concentrated in vacuo. The residue was quenched with sat. NaHCO3 solution and the aqueous phase was extracted with EtOAc (25 ml, ×2). The combined organic phase was dried (Na2SO4) and concentrated in vacuo. The crude residue was purified by column chromatography with n-hexane/DCM (80:20) to give the title compound (130 mg, 59.63%).

1. temperatureAfter cooling
2. concentrationthe mixture was concentrated in vacuo
3. customThe residue was quenched with sat. NaHCO3 solution
4. extractionthe aqueous phase was extracted with EtOAc (25 ml, ×2)
5. dry with materialThe combined organic phase was dried (Na2SO4)
6. concentrationconcentrated in vacuo
7. customThe crude residue was purified by column chromatography with n-hexane/DCM (80:20)