反应详情

温度

100 °C

Sodium hydride (3.3 g of a 50% suspension in mineral oil, 69 mmol) was added to a solution of 4-mercaptopyridine (8.12 g, 73 mmol) in DMF (100 ml) and the mixture stirred for 30 minutes. 7-Fluoro-3,4-dihydroquinazolin-4-one (1.5 g, 9 mmol) was added and the reaction heated at 100° C. for 4 hours. The mixture was allowed to cool, diluted with water and extracted with ethyl acetate. The organic extracts were washed with water and brine, dried (MgSO4) and the solvent removed by evaporation. The residue was purified by column chromatography eluting with methylene chloride/methanol (97/3) to give 7-(4-pyridylthio)-3,4-dihydroquinazolin-4-one (500 mg, 6%).

1. temperatureto cool
2. extractionextracted with ethyl acetate
3. washThe organic extracts were washed with water and brine
4. dry with materialdried (MgSO4)
5. customthe solvent removed by evaporation
6. customThe residue was purified by column chromatography
7. washeluting with methylene chloride/methanol (97/3)