反应详情

N,N-Dimethyl-1,3-phenylenediamine dihydrochloride (5 mmol, 1.0 g), 2-benzoyl-4-oxo-pentanoic acid ethyl ester (5 mmol, 1.2 g), triethylamine (10 mmol, 10 g), and tosic acid (0.1 g) were combined in ethanol, then heated under reflux. The resulting oil was resuspended in methylene chloride, then washed with water, 5% sodium bicarbonate, and brine. The organic layer was dried over NaSO4, then the solids were separated and the solvents removed under vacuum. The crude material was purified over silica gel and yielded the named product (m.p. 111.7° C.-114° C.).

1. temperatureheated
2. temperatureunder reflux
3. washwashed with water, 5% sodium bicarbonate, and brine
4. dry with materialThe organic layer was dried over NaSO4
5. customthe solids were separated
6. customthe solvents removed under vacuum
7. customThe crude material was purified over silica gel