反应详情

A solution of 2-(methylthio)pyrido[3,4-d]pyrimidin-8(7H)-one (Preparation 32, 1.47 g, 7.61 mmol) in POCl3 (70 mL) was heated to 70° C. for 18 hours. The reaction was concentrated under reduced pressure and partitioned between EtOAc and saturated aqueous NaHCO3 solution. The aqueous layer was extracted with EtOAc and the combined organic layers were washed with water and brine, dried and concentrated. The residue was purified by silica gel column chromatography eluting with 0 to 20% EtOAc in cyclohexane to give the title compound (1.39 g, 86%).

1. concentrationThe reaction was concentrated under reduced pressure
2. custompartitioned between EtOAc and saturated aqueous NaHCO3 solution
3. extractionThe aqueous layer was extracted with EtOAc
4. washthe combined organic layers were washed with water and brine
5. customdried
6. concentrationconcentrated
7. customThe residue was purified by silica gel column chromatography
8. washeluting with 0 to 20% EtOAc in cyclohexane