反应详情

温度

100 °C

A mixture of 6-(2-furyl)-4,5-dihydro-3H-pyrrolo[3,2-d]pyrimidin-4-one (2.20 g) and phosphoryl chloride (10.7 g) was stirred at 100° C. for 20 min, dioxane (30 mL) was added, and the mixture was stirred at 100° C. for 3 hrs. After concentration under reduced pressure, saturated aqueous sodium hydrogen carbonate was added to the residue, and the mixture was extracted with ethyl acetate-acetone (155 mL×4). The organic layers were combined, washed with saturated brine (100 mL), dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue washed with ethyl acetate-diethyl ether, and dried under reduced pressure at 60° C. to give the title compound (2.19 g).

1. stirringthe mixture was stirred at 100° C. for 3 hrs
2. concentrationAfter concentration under reduced pressure, saturated aqueous sodium hydrogen carbonate
3. additionwas added to the residue
4. extractionthe mixture was extracted with ethyl acetate-acetone (155 mL×4)
5. washwashed with saturated brine (100 mL)
6. dry with materialdried over anhydrous magnesium sulfate
7. concentrationconcentrated under reduced pressure
8. washThe residue washed with ethyl acetate-diethyl ether
9. customdried under reduced pressure at 60° C.