反应详情

A solution of 5-bromo-3-methyl-benzene-1,2-diamine (Maybridge, 3 g; 14.92 mmol) in formic acid (75 mL) was heated at reflux for 16 hours. Reaction mixture was concentrated under vacuum to give a brown oil. It was extracted by EtOAc from a saturated aqueous solution of NaHCO3, dried over MgSO4 and evaporated under vacuum to give the title compound as a pale yellow solid (3.07 g, 97%). 1H NMR (DMSO-d6) δ 12.92-12.34 (bs, 1H), 8.22 (s, 1H), 7.59 (br s, 1H), 7.17 (s, 1H), 3.33 (s, 3H). LC/MS (Method B): 211.0 (M+H)+.

1. temperatureat reflux for 16 hours
2. customReaction mixture
3. concentrationwas concentrated under vacuum
4. customto give a brown oil
5. extractionIt was extracted by EtOAc from a saturated aqueous solution of NaHCO3
6. dry with materialdried over MgSO4
7. customevaporated under vacuum