反应详情

N,N-dimethyl-1,3-phenylenediamine dihydrochloride (5 mmol, 1.0 g), triethylamine (10 mmol, 1.4 mL), 3-oxo-2-(2-oxo-2-phenyl-ethyl)-butyric acid ethyl ester (5 mmol, 1.2 g), and tosic acid (0.1 g) were combined in ethanol (25 mL), then heated under reflux (12 hrs). The solvents were removed under vacuum, the resulting oil was redissolved in methylene chloride, then applied to a silica column. The purified product was collected as a translucent oil. The named compound was identified by 1H-NMR (CDCl3, ppm): 1.28 t (3H), 2.35 s (3H), 2.77 s (6H), 4.2 q (2H), 6.3-6.7 m (4H), and 7.0-7.3 m (5H).

1. temperatureheated
2. temperatureunder reflux (12 hrs)
3. customThe solvents were removed under vacuum
4. dissolutionthe resulting oil was redissolved in methylene chloride
5. customThe purified product was collected as a translucent oil