HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 1-{2-{-N-[4-(4-Fluorophenyl)-4-oxobutyl]-N-methylamino}ethyl}-4-(3-chlorophenoxy)piperidine dihydrochloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Tetrafluoro-m-phenylenediamine dihydrochloride | HCID 149026 | — |
| Reactant | 1-{2-{N-{3-[2-(4-Fluorophenyl)-1,3-dioxolan-2-yl]-propyl}-N-methylamino}ethyl}-4-(3-chlorophenoxy)piperidine dihydrochloride | HCID 20283078 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 1-{2-{-N-[4-(4-Fluorophenyl)-4-oxobutyl]-N-methylamino}ethyl}-4-(3-chlorophenoxy)piperidine dihydrochloride | HCID 20283044 | — |
Reaction Steps
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.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04518713 |
| Source dataset | uspto-grants-1985_05 |
| ORD ID | ord-8e6ea5049fa748f1adbf86de1906491d |
| Source note | uspto-grants-1985_05 |