反应详情

Ethyl 4-fluoro-2-(3-nitrophenylmethylene)-3-oxobutanoate (0.6 g, 2.1 mmoles) and ethyl 3,3-diamino-2-propenoate hydrochloride (0.34 g, 12.0 mmoles) were heated at reflux in ethanol (10 ml) and a solution of sodium (0.05 g) in ethanol (5 ml) was added over one hour. The resulting solution was heated at reflux for a further 10 minutes and then filtered hot. The ethanolic solution was evaporated to dryness in vacuo and the resulting solid triturated with 2-propanol. The resulting solid was chromatographed on silica eluting with ether/petroleum ether (60°-80°) mixtures to give pure title compound, mp 177°-8°.

1. temperatureThe resulting solution was heated
2. temperatureat reflux for a further 10 minutes
3. filtrationfiltered hot
4. customThe ethanolic solution was evaporated to dryness in vacuo
5. customthe resulting solid triturated with 2-propanol
6. customThe resulting solid was chromatographed on silica eluting with ether/petroleum ether (60°-80°)