反应详情

温度

100 °C

Nitric acid (10 ml) was added slowly to a solution of 7-(3,5-dimethyl-4-isoxazolyl)-4-quinolinol (for a preparation see Intermediate 14 (28 g, 104 mmol) in propanoic acid (450 ml) at room temperature, followed by heating the reaction mixture to 100° C. for 1 h. After cooling with an ice bath, the precipitate was filtered off, washed with pentane to give the title compound as a yellow powder (27 g, 82%). [APCI-MS] m/z: 314 [M−H]−, Rt 2.12 min. 1H NMR (300 MHz, DMSO-d6, ppm) δ: 13.06 (s, 1H), 9.26 (s, 1H), 7.84 (s, 1H), 7.67 (s, 1H), 3.98 (s, 3H), 2.39 (s, 3H), 2.19 (s, 3H).

1. customat room temperature
2. temperatureAfter cooling with an ice bath
3. filtrationthe precipitate was filtered off
4. washwashed with pentane