反应详情

温度

55 °C

2N Hydrochloric acid (6.0 ml) was added to an ethanol solution (18 ml) of 5-fluoro-8-methoxymethoxy-3-(4-methoxyphenyl)-1H-quinolin-4-one (350 mg, 1.06 mmol). The mixture was stirred at 55° C. for 1 hour. The stirred mixture was cooled to room temperature, and 1N sodium hydrate (11.6 ml) was added thereto to obtain a pH of 3 to 4. The mixture in which pH was adjusted was concentrated under reduced pressure, and the residue was then purified by silica gel column chromatography (dichloromethane:methanol=50:1→20:1). The purified product was concentrated under reduced pressure, and the residue was crystallized from ethanol, collected by filtration, washed with ethanol, and dried to thereby obtain 165 mg of powdery pale dark brown 5-fluoro-8-hydroxy-3-(4-methoxyphenyl)-1H-quinolin-4-one (yield: 54%).

1. temperatureThe stirred mixture was cooled to room temperature
2. customto obtain a pH of 3 to 4
3. concentrationThe mixture in which pH was adjusted was concentrated under reduced pressure
4. customthe residue was then purified by silica gel column chromatography (dichloromethane:methanol=50:1→20:1)
5. concentrationThe purified product was concentrated under reduced pressure
6. customthe residue was crystallized from ethanol
7. filtrationcollected by filtration
8. washwashed with ethanol
9. customdried