Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Sodium Carbonate | HCID 10340 | — |
| Edukt | 4-(4-Chloro-3-(trifluoromethyl)phenyl)piperidin-4-ol | HCID 89107 | — |
| Edukt | 807-24-9 | HCID 20366912 | — |
| Lösungsmittel | Toluene | HCID 1140 | — |
| Produkt | HCID 20366934 | HCID 20366934 | — |
Reaktionsschritte
A mixture of 4.1 g of 4,4-diphenylcyclohexyl tosylate, 2.8 g of 4-(4-chloro-3-trifluoromethylphenyl)-4-piperidinol, 1.1 g of sodium carbonate and 400 ml of toluene is stirred under reflux for 48 hours. The reaction mixture is concentrated completely under reduced pressure, water is added to the residue, and the aqueous mixture is extracted with chloroform. The extract is washed with water and dried over sodium sulfate, and the solvent is removed. The esidual viscous oil is purified by column chromatography on silica gel using chloroform and then chloroform - methanol (9:1) as an eluent. The purified base is converted in a conventional manner into the hydrochloride. Thus is obtained 1-(4,4-diphenylcyclohexyl)-4-(4-chloro-3-trifluoromethylphenyl)-4-piperidinol hydrochloride monohydrate as white crystals, melting at 270°-273° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US04076821 |
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| Quelldatensatz | uspto-grants-1978_02 |
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| ORD ID | ord-6b2e2ad3436c4cc69ba735545e7b983b |
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| Quellennotiz | uspto-grants-1978_02 |
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