反应详情

温度

90 °C

A mixture of 2-amino-5-benzyl-6-methylpyrimidine-4-ol (1.2 g, 5.57 mmol) and phosphorous oxychloride (9 ml) was kept to warm at 90° C. for 6 hours. The reaction mixture was concentrated in vacuo. Ice-water was added to the residue and an aqueous ammonia was cautiously added thereto. The solution was extracted with chloroform. The organic layer was washed with saturated brine, dried over sodium sulfate and concentrated in vacuo. The residue was purified by silica gel column chromatography (chloroform: ethyl acetate=8:2) to give the object compound (700 mg, 53.7%).

1. concentrationThe reaction mixture was concentrated in vacuo
2. additionIce-water was added to the residue
3. additionan aqueous ammonia was cautiously added
4. extractionThe solution was extracted with chloroform
5. washThe organic layer was washed with saturated brine
6. dry with materialdried over sodium sulfate
7. concentrationconcentrated in vacuo
8. customThe residue was purified by silica gel column chromatography (chloroform: ethyl acetate=8:2)