反应详情

4.0 g of 1-(2-chlorophenyl)-2-methoxyethylene are added dropwise within 20 minutes to 9.55 g of 5-nitrofurfurol in 12 cc of dry benzene at room temperature after the addition of one drop of diethyl ether/trifluoroborane. The mixture is stirred at 35°-40° for 1 hour and is then successively washed with a 5% aqueous sodium acetate solution and water, the benzene solution is dried over magnesium sulphate and concentrated by evaporation. The residue is taken up in 3 cc of concentrated hydrochloric acid, 17 cc of water and 120 cc of glacial acetic acid, and the mixture is stirred at 80°-85° for 3 hours. The mixture is concentrated in a vacuum, and, after cooling, the title compound is obtained as yellow crystals having a M.P. of 148°-151°.

1. washis then successively washed with a 5% aqueous sodium acetate solution and water
2. dry with materialthe benzene solution is dried over magnesium sulphate
3. concentrationconcentrated by evaporation
4. stirring17 cc of water and 120 cc of glacial acetic acid, and the mixture is stirred at 80°-85° for 3 hours
5. concentrationThe mixture is concentrated in a vacuum
6. temperatureafter cooling