反应详情

A solution of 5-bromo-2,3-diaminofluorobenzene (Apollo, 3 g; 14.63 mmol) in formic acid (75 mL) was heated at reflux overnight after which the reaction mixture was concentrated under vacuum to give a brown oil. 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 (2.91 g, 92%). 1H NMR (DMSO-d6): δ 8.30 (s, 1H), 7.62 (d, J=1.5 Hz, 1H), 7.27 (dd, J=10.3, 1.5 Hz, 2H), 3.32 (bs, 2H). HPLC (Method A), Rt: 2.09 min (purity: 97.4%). LC/MS (Method B): 216.9 (M+H)+.

1. temperatureat reflux overnight after which the reaction mixture
2. concentrationwas concentrated under vacuum
3. customto give a brown oil
4. extractionIt was extracted with EtOAc from a saturated aqueous solution of NaHCO3
5. dry with materialdried over MgSO4
6. customevaporated under vacuum