反应详情

温度

105 °C

A suspension of 2-hydroxy-3-methyl-5-naphthalen-2-yl-6-pyridin-4-yl-3H-pyrimidin-4-one (10.0 g, 30.4 mmol) and phosphorous oxychloride (250 mL, 3 mol) was heated to 105° C. for 6 h to form a solution. Monitoring reaction by HPLC showed ˜90% conversion. The reaction solution was cooled and the solvent removed under reduced pressure. Foam residue was dissolved in 500 mL 5% ethanol/chloroform. The organic layer was washed with 100 mL water three times and once with 100 mL 5% NaHCO3. Organic dried over magnesium sulfate, then dried onto 30 g of silica. Final product purified on 400 g silica eluting with 0 to 2.5% methanol/dichloromethane to give a yellow solid. M+1=348.

1. customto form a solution
2. customMonitoring reaction by HPLC
3. temperatureThe reaction solution was cooled
4. customthe solvent removed under reduced pressure
5. dissolutionFoam residue was dissolved in 500 mL 5% ethanol/chloroform
6. washThe organic layer was washed with 100 mL water three times and once with 100 mL 5% NaHCO3
7. dry with materialOrganic dried over magnesium sulfate
8. customdried onto 30 g of silica
9. customFinal product purified on 400 g silica eluting with 0 to 2.5% methanol/dichloromethane
10. customto give a yellow solid