反应详情

After refluxing a solution of 5-((3-(3-pyrrolidin-1-ylpropoxy)-4-methoxyanilino)methylene)-2,2-dimethyl-1,3-dioxane-4,6-dione (4.9 g, 12 mmol) in phenyl ether (50 ml) for 1 minute, the mixture was poured into petroleum ether (500 ml). The solid was collected by filtration and purified by reverse phase chromatography on a Diaion (trade mark of Mitsubishi) HP20SS resin column eluting with water/methanol (100/0 increasing to 20/80). After removal of the solvent by evaporation, the purified product was azeotroped with a mixture of ethanol and toluene to give 6-methoxy-7-(3-pyrrolidin-1-ylpropoxy)-1,4-dihydroquinolin-4-one (1 g, 27%).

1. filtrationThe solid was collected by filtration
2. custompurified by reverse phase chromatography on a Diaion (trade mark of Mitsubishi) HP20SS resin column
3. washeluting with water/methanol (100/0 increasing to 20/80)
4. customAfter removal of the solvent
5. customby evaporation
6. customthe purified product was azeotroped with a mixture of ethanol and toluene