反应详情

To a solution of 1-(4-aminophenyl)-3,4-dihydrocarbostyril (0.45 g) in dichloromethane (15 ml) is added triethylamine (0.29 g). Thereto is added 2,4-dimethoxybenzoyl chloride (0.42 g) with stirring under ice cooling. The mixture is refluxed with heating for 0.5 hour. After cooling, water is added thereto and the mixture is extracted with dichloromethane, washed with water and then dried with magnesium sulfate. The solvent is distilled off under reduced pressure and the residue is purified by silica gel column chromatography and recrystallized from ethanol/diethyl ether/n-hexane to give 1-[4-(2,4-dimethoxybenzoylamino)phenyl]-3,4-dihydrocarbostyril (0.44 g) as white powder, m.p.: 226°-227° C.

1. temperatureThe mixture is refluxed
2. temperaturewith heating for 0.5 hour
3. temperatureAfter cooling
4. extractionthe mixture is extracted with dichloromethane
5. washwashed with water
6. dry with materialdried with magnesium sulfate
7. distillationThe solvent is distilled off under reduced pressure
8. customthe residue is purified by silica gel column chromatography
9. customrecrystallized from ethanol/diethyl ether/n-hexane