反应详情

To 1.00 g (4.83 mmol) of 6-nitroquinazoline-2,4 (1H,3H)-dione were added 32.90 g (0.22 mol) of phosphorus oxychloride and 0.70 ml (4.83 mmol) of diisopropylformamide, and the resulting mixture was subjected to heating under reflux for 24 hours. After phosphorus oxychloride was removed in vacuo, the mixture was dissolved in 15 ml of acetonitrile, followed by addition of 2.49 ml (29.11 mmol) of isopropylamine under ice cooling and stirring under ice cooling for 30 minutes. To the reaction solution was added water, followed by extraction with ethyl acetate, washing with brine and drying over anhydrous sodium sulfate. After the solvent was distilled off, the residue was purified by a silica gel column to give 870 mg (yield: 67.5%) of the title compound.

1. temperatureto heating
2. temperatureunder reflux for 24 hours
3. customAfter phosphorus oxychloride was removed in vacuo
4. dissolutionthe mixture was dissolved in 15 ml of acetonitrile
5. extractionfollowed by extraction with ethyl acetate
6. washwashing with brine
7. dry with materialdrying over anhydrous sodium sulfate
8. distillationAfter the solvent was distilled off
9. customthe residue was purified by a silica gel column