反应详情

A mixture of 1-methyl-2-nitro-vinylamine (1 g), 5-propylcyclohexane-1,3-dione (1.61 g) and 3-bromo-5-ethoxy-4-hydroxy-benzaldehyde (2.57 g) in ethanol (50 ml) was stirred at reflux for 17 h. The reaction mixture was concentrated in vacuo. The residue was dissolved in dichloromethane. A precipitate formed, which was collected by filtration. The solid was chromatographed on silicagel in heptane/EtOAc (from 1/0 to 0/1) as eluent. Yield: 2.8 g. MS-ESI: [M+H]+=465.0/467.0

1. temperatureat reflux for 17 h
2. concentrationThe reaction mixture was concentrated in vacuo
3. dissolutionThe residue was dissolved in dichloromethane
4. customA precipitate formed
5. filtrationwhich was collected by filtration
6. customThe solid was chromatographed on silicagel in heptane/EtOAc (from 1/0 to 0/1) as eluent