反应详情

温度

90 °C

A mixture of 5-nitro-2-phenyl-4(3H)-pyrimidinone (6 g) and phosphorus oxychloride (8.5 g) is stirred at 90° C. for four hours. After cooling, the reaction mixture is concentrated under reduced pressure, and the residue is dissolved in chloroform. To the mixture is added ice-water, and the mixture is stirred. The mixture is neutralized with 1N aqueous sodium hydroxide solution, and the chloroform layer is separated, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue is recrystallized from ethanol to give the desired compound (5.6 g).

1. temperatureAfter cooling
2. concentrationthe reaction mixture is concentrated under reduced pressure
3. dissolutionthe residue is dissolved in chloroform
4. additionTo the mixture is added ice-water
5. stirringthe mixture is stirred
6. customthe chloroform layer is separated
7. dry with materialdried over anhydrous sodium sulfate
8. concentrationconcentrated under reduced pressure
9. customThe residue is recrystallized from ethanol