HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 1-{3-{N-[4-(4-Fluorophenyl)-4-oxobutyl]-N-methylamino}propyl}-4-(3-chlorophenoxy)piperidine dihydrochloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 20283103 | HCID 20283103 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 1-{3-{N-[4-(4-Fluorophenyl)-4-oxobutyl]-N-methylamino}propyl}-4-(3-chlorophenoxy)piperidine dihydrochloride | HCID 20283110 | 161.4% |
Reaction Steps
A solution prepared from 3.36 g (5.96 mmol) of 1-{3-{N-{3-[2-(4-fluorophenyl)-1,3-dioxolan-2-yl]propyl}-N-methylamino}propyl}-4-(3-chlorophenoxy)piperidine dihydrochloride, 90 ml of methanol and 40 ml of 3N HCl was heated at reflux under nitrogen for 3 hours. The solution was allowed to cool to room temperature, neutralized with saturated sodium bicarbonate and the methanol evaporated. The residue was made basic with sodium carbonate, extracted twice with ether and washed with saturated sodium chloride. The ether solution was dried over potassium carbonate. Filtration followed by evaporation of the solvent provided an oil. The dihydrochloride was recrystallized from ethanol/methanol to provide 2.50 g (74.4%) of the desired ketone.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04518713 |
| Source dataset | uspto-grants-1985_05 |
| ORD ID | ord-51ab6d5b452d41dd98caf5a1024c5777 |
| Source note | uspto-grants-1985_05 |