反应详情

温度

110 °C

A mixture of ethyl 4-(4-oxo-4,5-dihydro-3H-pyrrolo[3,2-d]pyrimidin-6-yl)benzoate (2.97 g) and phosphoryl chloride (16.45 g) was stirred at 110° C. for 1 hr, dioxane (10 mL) was added and the mixture was heated under reflux for 4 hrs. After concentration under reduced pressure, ethanol (30 mL) was added to the residue and, after stirring at room temperature for 30 min, the precipitated solid was collected by filtration. The solid was washed with ethanol and dried under reduced pressure at 60° C. to give the title compound (3.34 g).

1. temperaturethe mixture was heated
2. temperatureunder reflux for 4 hrs
3. concentrationAfter concentration under reduced pressure, ethanol (30 mL)
4. additionwas added to the residue
5. stirringafter stirring at room temperature for 30 min
6. filtrationthe precipitated solid was collected by filtration
7. washThe solid was washed with ethanol
8. customdried under reduced pressure at 60° C.