反应详情

温度

100 °C

3,4-Diaminobenzonitrile (1.0 g; 7.5 mmol) was dissolved in formic acid (3 mL) and heated at 100° C. for 1.5 hours. The mixture was cooled, neutralised with 10% sodium hydroxide and the resulting precipitate isolated by filtration and dried in vacuo to yield the title compound as a brown solid (890 mg; 82%). 1H NMR (DMSO-d6) δ 8.50 (1H, s), 8.19 (1H, s), 7.79 (1H, d, J=8.3 Hz), 7.62 (1H, dd, J=8.3, 1.54 Hz). LC/MS (Method C): 144 (M+H)'. HPLC (Method F) Rt=2.14 min (Purity: 99.4%).

1. temperatureThe mixture was cooled
2. customthe resulting precipitate isolated by filtration
3. customdried in vacuo