反应详情

3-Nitrobenzaldehyde (1.51 g, 10 mmoles), ethyl 4-fluoro-3-oxo-butanoate (3 g, 20 mmoles) and aqueous ammonia (1.1 ml, d=0.88) in ethanol (15 ml) were heated at reflux for 14 hours more aqueous ammonia (0.55 ml) was added after 6 hours. The solvent was removed in vacuo and the residue was chromatographed on silica eluting with ether/petroleum ether (60°-80°) mixtures and the product obtained was recrystallised from 2-propanol to give the title compound as yellow crystals (0.4 g) mp 113°-4°.

1. additionwas added after 6 hours
2. customThe solvent was removed in vacuo
3. customthe residue was chromatographed on silica eluting with ether/petroleum ether (60°-80°) mixtures
4. customthe product obtained
5. customwas recrystallised from 2-propanol