反应详情

6.4 g of 1-(4-benzyloxyphenyl)-2-methoxyethylene, diluted with 10 cc of benzene, are added dropwise at 0°-5° to 11.15 g of 5-nitrofuran-2-aldehyde in 30 cc of dry benzene after the addition of a few drops of diethyl ether/trifluoroborane. The mixture is stirred at 40° for 11/2 hours, is washed with a 5% aqueous sodium acetate solution and with water, dried with magnesium sulphate and concentrated by evaporation. The residue is heated to 90° for 4 hours with 10% hydrochloric acid and glacial acetic acid. The mixture is again concentrated by evaporation, is taken up in ether and the acid salt portion is filtered off. After concentration, orange crystals having a M.P. of 145°-155°, crystallize from the ether solution.

1. washis washed with a 5% aqueous sodium acetate solution and with water
2. dry with materialdried with magnesium sulphate
3. concentrationconcentrated by evaporation
4. temperatureThe residue is heated to 90° for 4 hours with 10% hydrochloric acid and glacial acetic acid
5. concentrationThe mixture is again concentrated by evaporation
6. filtrationthe acid salt portion is filtered off
7. concentrationAfter concentration, orange crystals
8. customcrystallize from the ether solution