反应详情

温度

55 °C

A mixture of 0.09 g of methyl (3RS,4RS)-4-[3-(R,S)-amino-3-(3-fluoro-6-methoxyquinolin-4-yl)propyl]-1-[2-(2,5-difluorophenylthio)ethyl]piperidine-3-acetate in 0.36-cm3 of a 1 N aqueous sodium hydroxide solution and 3-cm3 of dioxane was heated at a temperature in the region of 55° C., with stirring and under an inert atmosphere, for 4 hours. After cooling in the vicinity of 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 5-cm3 of distilled water and acidified with a 1-N aqueous hydrochloric acid solution and was concentrated. The aqueous phase was washed with 8-cm3 of dichloromethane and then concentrated according to the conditions described above. The residue obtained was taken up in 10-cm3 of acetone and then it was filtered on sintered glass. 0.081 g of (3RS,4RS)-4-[3-(R,S)-amino-3-(3-fluoro-6-methoxyquinolin-4-yl)propyl]-1-[2-(2,5-difluorophenylthio)ethyl]piperidine-3-acetic acid hydrochloride wereobtained in the form of a white solid.

1. temperatureAfter cooling in the vicinity of 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. concentrationwas concentrated
5. washThe aqueous phase was washed with 8-cm3 of dichloromethane
6. concentrationconcentrated
7. customThe residue obtained
8. filtrationit was filtered on sintered glass