反应详情

温度

50 °C

2N hydrochloric acid (6.3 ml) was added to an ethanol solution (20 ml) of ethyl (5-fluoro-4-oxo-8-propoxy-3-{4-[2-(tetrahydropyran-2-yloxy)ethoxy]phenyl}-4H-quinolin-1-yl)acetate (840 mg, 1.59 mmol) and stirred at 50° C. for 2 hours. The resulting mixture was cooled to room temperature and then concentrated under reduced pressure. Ethyl acetate and water were added to the residue, followed by separation. The thus-obtained organic layer was washed with an aqueous saturated sodium chloride solution, and then concentrated under reduced pressure. The residue was purified using silica gel column chromatography (dichloromethane:methanol=30:1→15:1). The purified product was concentrated under reduced pressure, giving a pale yellow oily substance of ethyl{5-fluoro-3-[4-(2-hydroxyethoxy)phenyl]-4-oxo-8-propoxy-4H-quinolin-1-yl}acetate (627 mg, yield: 89%).

1. temperatureThe resulting mixture was cooled to room temperature
2. concentrationconcentrated under reduced pressure
3. additionEthyl acetate and water were added to the residue
4. customfollowed by separation
5. washThe thus-obtained organic layer was washed with an aqueous saturated sodium chloride solution
6. concentrationconcentrated under reduced pressure
7. customThe residue was purified
8. concentrationThe purified product was concentrated under reduced pressure