反应详情

To a solution of 1,2,3,4-tetrahydroquinoline (28.7 g) in acetone (400 ml) and water (200 ml) is added potassium carbonate (38.8 g) and further thereto is added 4-benzoylaminobenzoyl chloride (56 g) under ice-cooling. The mixture is stirred at room temperature overnight. Water is added to the reaction mixture, and the mixture is extracted with dichloromethane. The extract is dried over magnesium sulfate, and the solvent is distilled off under reduced pressure. The resulting residue is purified by silica gel column chromatography and recrystallized from methanol to give 1-[4-(benzoylamino)benzoyl]-1,2,3,4-tetrahydroquinoline (57 g) as white powder, m.p. 202.5°-203.5° C.

1. temperaturecooling
2. extractionthe mixture is extracted with dichloromethane
3. dry with materialThe extract is dried over magnesium sulfate
4. distillationthe solvent is distilled off under reduced pressure
5. customThe resulting residue is purified by silica gel column chromatography
6. customrecrystallized from methanol