反应详情

To a solution of 4-aminobenzonitrile (5.1 g, 43 mmol) in dry methanol (60 mL) at 0 C, hydrogen chloride gas was bubbled through until saturation was reached. The mixture was then stirred at room temperature overnight. It was concentrated in vacuo. The residue was dissolved in dry methanol (60 mL). To the solution, N-methyl ethylenediamine (19 mL, 216 mmol) was added. The mixture was then heated to reflux for 3 h. After being cooled in fridge overnight, the precipitated product was collected by filtration, then was dried on vacuum to give white solids (3.7 g). MS 176.0 (M+H).

1. concentrationIt was concentrated in vacuo
2. dissolutionThe residue was dissolved in dry methanol (60 mL)
3. temperatureThe mixture was then heated
4. temperatureto reflux for 3 h
5. temperatureAfter being cooled in fridge overnight
6. filtrationthe precipitated product was collected by filtration
7. customwas dried on vacuum