HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 2-[3-(3,4-Dichlorophenyl)piperidin-3-yl]ethanol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 3-(2-Tetrahydropyranyloxyethyl)-3-(3,4-dichlorophenyl)piperidine | HCID 21197691 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Ether isopropyl ether | HCID 21919906 | — |
| Product | 2-[3-(3,4-Dichlorophenyl)piperidin-3-yl]ethanol | HCID 15460400 | 106.9% |
Reaction Steps
A saturated solution of hydrogen chloride in ether is added to a solution of 55 g of 3-(2-tetrahydropyranyloxyethyl)-3-(3,4-dichlorophenyl)piperidine in 200 ml of methanol until the pH is 1. The mixture is stirred for half an hour at room temperature and concentrated to dryness, the residue is taken up in water, rendered alkaline with a solution of NaOH and extracted with CH2Cl2 and the extract is washed with a saturated solution of. NaCl, dried over Na2SO4 and evaporated to dryness to give an oil. This oil is taken up in 200 ml of an isopropyl ether/ether mixture (50/50 v/v). After stirring and filtration, the product is washed with ethyl ether and dried under vacuum over P2O5 to give 45 g of the expected product. M.p.=22° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05554763 |
| Source dataset | uspto-grants-1996_09 |
| ORD ID | ord-109334a696ed47129d5cbe852783e924 |
| Source note | uspto-grants-1996_09 |