反应详情

A solution of 3,4-diaminobenzonitrile (1 g; 7.51 mmol) in formic acid (40 mL) was heated at reflux for 3 hours then concentrated in vacuo to give a brown oily residue. It was extracted with EtOAc from a saturated aqueous solution of NaHCO3, dried over MgSO4 and evaporated under vacuum to give the title compound as a light pink solid (1.05 g, 98%). 1H NMR (DMSO-d6): δ 12.97 (br s, 1H), 8.48 (s, 1H), 8.16 (d, J=0.8 Hz, 1H), 7.76 (d, J=8.3 Hz, 1H), 7.59 (dd, J=8.3, 1.5 Hz, 1H). LC/MS (Method B): 144.1 (M+H)+.

1. temperatureat reflux for 3 hours
2. concentrationthen concentrated in vacuo
3. customto give a brown oily residue
4. extractionIt was extracted with EtOAc from a saturated aqueous solution of NaHCO3
5. dry with materialdried over MgSO4
6. customevaporated under vacuum