反应详情

To 1 mL of an ethanol solution containing 0.10 g of ethyl 1-(2,3-dihydro-1,4-benzodioxin-6-ylmethyl)-4-(3-(7-methoxy-2-oxoquinolin-1(2H)-yl)propyl)piperidine-4-carboxylate, 0.15 mL of 20% aqueous sodium hydroxide solution was added and refluxed with heating for 2 hours. Then, more 0.10 mL of 20% aqueous sodium hydroxide solution was added and refluxed with heating for 5 hours. After left to stand at room temperature overnight, the solvent was removed under reduced pressure, water was added, and adjusted to pH 6.7 with 6.0 mol/L hydrochloric acid. The solvent was removed under reduced pressure, and the residue thus obtained was purified by reversed-phase silica gel column chromatography [eluent; acetonitrile:water=3:7] to give 21 mg of 1-(2,3-dihydro-1,4-benzodioxin-6-ylmethyl)-4-(3-(7-methoxy-2-oxoquinolin-1(2H)-yl)propyl)piperidine-4-carboxylic acid as a white solid.

1. additionwas added
2. temperaturerefluxed
3. temperaturewith heating for 2 hours
4. temperaturerefluxed
5. temperaturewith heating for 5 hours
6. waitAfter left
7. customthe solvent was removed under reduced pressure, water
8. additionwas added
9. customThe solvent was removed under reduced pressure
10. customthe residue thus obtained
11. customwas purified by reversed-phase silica gel column chromatography [eluent; acetonitrile:water=3:7]