Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Sodium Iodide | HCID 5238 | — |
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | Sodium Bicarbonate | HCID 516892 | — |
| Edukt | 4-Bromo-1,1,1-trifluorobutane | HCID 521006 | — |
| Edukt | 1-[2-(3,3,5,5-Tetramethylcyclohexyl)phenyl]piperazine | HCID 11992284 | — |
| Lösungsmittel | Diethyl Ether | HCID 3283 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | HCID 23142083 | HCID 23142083 | — |
Reaktionsschritte
A mixture of the 1-[2-(3,3,5,5-tetramethylcyclohexyl)phenyl]piperazine (30 mg, 0.1 mmol) produced in Example (8b), 1-bromo-4,4,4-trifluorobutane (24.4 mg, 0.125 mmol), sodium iodide (1.5 mg, 0.01 mmol), potassium carbonate (20.8 mg, 0.15 mmol) and dimethylformamide (1 mL) was stirred for 2 hours and 30 minutes at an external temperature of 60° C. Aqueous solution of sodium hydrogencarbonate was added to the reaction mixture and extraction was performed with diethyl ether. The solvent was distilled off by nitrogen stream to the separated organic layer. The resultant residue was purified by NH silica gel column chromatography (ethyl acetate/heptane) to give 1-[2-(3,3,5,5-tetramethylcyclohexyl)phenyl]-4-(4,4,4-trifluorobutyl)piperazine.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US07425554B2 |
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| Quelldatensatz | uspto-grants-2008_09 |
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| ORD ID | ord-0d4644e28c5c45b0abd9445564cf8337 |
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| Quellennotiz | uspto-grants-2008_09 |
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