反应详情

A mixture of ethyl 2-bromopropionate (0.64 g), 4-[N-(7-chloroisoquinolin-3-yl)-N-methylamino]phenol (0.92 g), anhydrous potassium carbonate (0.49 g) and methyl ethyl ketone was heated under reflux for a period of 5 hours. The solution was cooled, washed with water, and dried over anhydrous magnesium sulfate. The solvent was removed by distillation under reduced pressure and the product was purified by column chromatography over silica gel (eluant dichloromethane) to give ethyl 2-{4-[N-(7-chloroisoquinolin-3-yl)-N-methylamino]phenoxy}propionate (1.00 g) as a green oil. The assigned structure was confirmed by proton magnetic resonance spectroscopy and mass spectrometry. Proton magnetic resonance spectrum (CDCl3 ; δ in ppm): 1.25 (3H, t); 1.60 (3H, d); 3.45 (3H, s); 4.22 (2H, q); 4.75 (1H, q); 6.52 (1H, s); 6.8-7.4 (6H, m); 7.62 (1H, m); 8.75 (1H, s).

1. temperaturewas heated
2. temperatureunder reflux for a period of 5 hours
3. temperatureThe solution was cooled
4. washwashed with water
5. dry with materialdried over anhydrous magnesium sulfate
6. customThe solvent was removed by distillation under reduced pressure
7. customthe product was purified by column chromatography over silica gel (eluant dichloromethane)