反应详情

800 ml of acetonitrile was added to 70.0 g (0.40 mol) of 4-methoxybenzylamine hydrochloride and 39.5 g (0.44 mol) of sodium dicyanamide. The mixture was refluxed for 19 hours, and the solvent was distilled off under reduced pressure. The residue was heated and dissolved in methanol, and insolubles were filtered off. The solvent was distilled off under reduced pressure, and the residue was recrystallized from ethyl acetate to obtain 67.0 g of colorless crystals having a melting point of 89 to 92° C.

1. temperatureThe mixture was refluxed for 19 hours
2. distillationthe solvent was distilled off under reduced pressure
3. temperatureThe residue was heated
4. dissolutiondissolved in methanol
5. filtrationinsolubles were filtered off
6. distillationThe solvent was distilled off under reduced pressure
7. customthe residue was recrystallized from ethyl acetate