反应详情

A solution prepared from 8.55 g (15.5 mmol) of 1-{2-{N-{3-[2-(4-fluorophenyl)-1,3-dioxolan-2-yl]propyl}-N-methylamino}ethyl}-4-(3-chlorophenoxy)piperidine dihydrochloride, 130 ml of methanol and 50 ml of 3N HCl was heated at reflux for 3 hours under nitrogen and allowed to cool to room temperature. The methanol was evaporated and the residue made basic with saturated sodium carbonate and extracted with ether. The ether extract was washed with saturated sodium chloride and dried over potassium carbonate. Filtration followed by evaporation of the solvent provided an oil. The yield of the dihydrochloride was 6.8 g (13.4 mmol, 86%). Recrystallization from ethanol/methanol provided analytically pure material.

1. temperaturewas heated
2. temperatureat reflux for 3 hours under nitrogen
3. customThe methanol was evaporated
4. extractionextracted with ether
5. extractionThe ether extract
6. washwas washed with saturated sodium chloride
7. dry with materialdried over potassium carbonate
8. filtrationFiltration
9. customfollowed by evaporation of the solvent
10. customprovided an oil
11. customRecrystallization from ethanol/methanol
12. customprovided analytically pure material