反应详情

温度

60 °C

A mixture of 7-(2,3-epoxypropoxy)flavone (15 g, 51.0 mmol) and N-(3-nicotinylpropyl)benzylamine (22.5 g, 100 mmol) in ethanol (150 ml) was heated at 60° C. for 3 hours. The ethanol was then evaporated and the residue was washed with cyclohexane (three times) to remove the excess amine. The remaining residue was then extracted with ethyl acetate (twice), and the extracts were evaporated to give a red syrup. Purification of the red syrup by flash column chromatography eluting with EtOAc--MeOH (20:1) gave 8.0 g of a yellow syrup, 30% yield, which is stored in the refrigerator and used for the further reaction.

1. customThe ethanol was then evaporated
2. washthe residue was washed with cyclohexane (three times)
3. customto remove the excess amine
4. extractionThe remaining residue was then extracted with ethyl acetate (twice), and the extracts
5. customwere evaporated
6. customto give a red syrup
7. customPurification of the red syrup by flash column chromatography
8. washeluting with EtOAc--MeOH (20:1)