反应详情

温度

75 °C

2N Sodium hydroxide (506 mL, 1011.43 mmol) was added to a stirred suspension of ethyl 6-bromo-4-oxo-1H-quinoline-3-carboxylate (59.9 g, 202.29 mmol) in EtOH (590 mL) and the resulting solution stirred at 75° C. for 1.5 h. Water was added and the mixture cooled to 0° C. The pH of the solution was adjusted to 3 using hydrochloric acid and the precipitate collected by filtration. The solid was washed with water, EtOH/water (1:1) then Et2O before being dried to afford the desired material (51.9 g, 96%) as a beige solid. NMR Spectrum: 1H NMR (500 MHz, DMSO-d6) δ 7.80 (1H, d), 8.05 (1H, d), 8.37 (1H, s), 8.93 (1H, s). Mass Spectrum: m/z (ES+)[M+H]+=270.

1. temperaturethe mixture cooled to 0° C
2. filtrationthe precipitate collected by filtration
3. washThe solid was washed with water, EtOH/water (1:1)
4. dry with materialEt2O before being dried