反应详情

温度

80 °C

To the mixture of hydroxylamine hydrochloride (42 mg, 0.6 mmol) and KOH (34 mg, 0.6 mmol) in EtOH (2 mL) was added the crude (Z)-1,7-dimethyl-3-(2-methyl-5-(1-(methylthio)-3-oxo-3-(thiazol-2-yl)prop-1-enyl amino)phenyl)-1,6-naphthyridin-2(1H)-one 32. The resulting mixture was heated at 80° C. for 30 min. Then NaOEt (40.8 mg, 0.6 mmol) was added and the reaction mixture was refluxed for 1 h. The mixture was purified by preparative LC/MS to give 1,7-dimethyl-3-(2-methyl-5-(3-(thiazol-2-yl)isoxazol-5-ylamino)phenyl)-1,6-naphthyridin-2(1H)-one (F1). 1H NMR (400 MHz, d6-DMSO) δ 9.50 (s, 1H), 9.13 (s, 1H), 7.95-8.10 (m, 3H), 7.88 (s, 1H), 7.38 (s, 1H), 7.30 (d, J=8.0 Hz, 1H), 7.18 (d, J=8.0 Hz, 1H), 6.94 (s, 1H), 3.65 (s, 1H), 2.72 (s, 3H), 2.03 (s, 3H). MS m/z 430.1 (M+1).

1. temperaturethe reaction mixture was refluxed for 1 h
2. customThe mixture was purified by preparative LC/MS