反应详情

A mixture of N-[3-methoxy-4-(4-methyl-imidazol-1-yl)-phenyl]-guanidine dinitrate (185 mg, 0.5 mmol), crude ethyl 3-dimethylamino-2-(4-chloro-benzoyl)-acrylate (292 mg, 1.0 mmol), and triethylamine (0.66 mL, 4.7 mmol) in ethanol (2 mL) was heated at reflux for 15 h. The mixture was cooled and diluted with ethyl acetate (50 mL). The solution was washed with sat. sodium carbonate solution (5 mL) and with brine (5 mL), dried over sodium sulfate and evaporated under reduced pressure. The residual material was purified by chromatography on silica gel using dichloromethane/0-20% methanol as eluent to give the title compound (157 mg, 68%) as a pale-yellow solid. Mp 216-218° C.

1. temperaturewas heated
2. temperatureat reflux for 15 h
3. temperatureThe mixture was cooled
4. washThe solution was washed with sat. sodium carbonate solution (5 mL) and with brine (5 mL)
5. dry with materialdried over sodium sulfate
6. customevaporated under reduced pressure
7. customThe residual material was purified by chromatography on silica gel