反应详情

温度

60 °C

A mixture of 0.355 g of methyl (3RS,4RS)-4-[3-(R,S)-amino-3-(3-fluoro-6-methoxyquinolin-4-yl)propyl]-1-[2-(2-thienylthio)ethyl]piperidine-3-acetate in 1.66-cm3 of a 1 N aqueous sodium hydroxide solution and 5-cm3 of dioxane was heated at a temperature in the region of 60° C., with stirring, for 2 hours. After cooling to about 20° C., the reaction mixture was concentrated to dryness under reduced pressure (2 kPa) at a temperature in the region of 50° C. The evaporation residue obtained was taken up in 30-cm3 of water and 30-cm3 of diethyl ether, the aqueous phase was separated after settling out and neutralized with 1.66-cm3 of a 1 N aqueous hydrochloric acid solution and was then extracted twice with 100-cm3 of ethyl acetate. The organic phase was dried over magnesium sulfate, filtered and then concentrated to dryness according to the same conditions above. 0.238 g of (3RS,4RS)-4-[3-(R,S)-amino-3-(3-fluoro-6-methoxyquinolin-4-yl)propyl]-1-[2-(2-thienylthio)ethyl]piperidine-3-acetic acid were obtained in the form of a white solid.

1. temperatureAfter cooling to about 20° C.
2. concentrationthe reaction mixture was concentrated to dryness under reduced pressure (2 kPa) at a temperature in the region of 50° C
3. customThe evaporation residue obtained
4. custom30-cm3 of diethyl ether, the aqueous phase was separated
5. extractionwas then extracted twice with 100-cm3 of ethyl acetate
6. dry with materialThe organic phase was dried over magnesium sulfate
7. filtrationfiltered
8. concentrationconcentrated to dryness