反应详情

温度

66 °C

4-(benzyloxy)-2-(1H-pyrazol-1-yl)pyrimidine-5-carboxylic acid, 2-e, (200 mg, 0.68 mmol) was dissolved in THF (20 ml) and treated with Et3N (204 mg, 2.02 mmol) and DPPA (204 mg, 0.74 mmol). The mixture was heated at 66° C. for 12 hours. Then water was added and the resulting mixture was continued to stir at reflux for 2 h. After that the mixture was concentrated under vacuum. The residue was diluted with aq. K2CO3 followed by extraction with ethyl acetate. The organic layer was dried over sodium sulfate and concentrated under vacuum. The residue was purified on silica gel column with the eluent of dichloromethane/methanol=50/1 (Rf=0.7) to provide compound 2-f (72 mg, 40%).

1. temperatureat reflux for 2 h
2. concentrationAfter that the mixture was concentrated under vacuum
3. additionThe residue was diluted with aq. K2CO3
4. extractionfollowed by extraction with ethyl acetate
5. dry with materialThe organic layer was dried over sodium sulfate
6. concentrationconcentrated under vacuum
7. customThe residue was purified on silica gel column with the eluent of dichloromethane/methanol=50/1 (Rf=0.7)