反应详情

To a mixture of 3-(4-(trifluoromethoxy)phenyl)isoxazole-5-carbohydrazide (2.4 g, 8.5 mmol) and acetimidamide hydrochloride (1.2 g, 12.8 mmol) in dry THF (60 mL), was added NaOH (512 mg, 12.8 mmol). The mixture was then refluxed for 16 h, then cooled to RT and concentrated under reduced pressure. The residue was purified by silica gel chromatography to afford the title compound as a white solid (1.9 g, 71%). 1H NMR (500 MHz, DMSO-d6) δ 8.12 (d, J=7.2 Hz, 2H), 7.58 (s, 1H). 7.54 (d, J=6.4 Hz, 2H), 2.46 (s, 3H). MS (ES+) C13H9F3N4O2 requires: 310. found: 311 [M+H]+.

1. temperatureThe mixture was then refluxed for 16 h
2. concentrationconcentrated under reduced pressure
3. customThe residue was purified by silica gel chromatography