Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Piperazine | HCID 4837 | — |
| Edukt | 4-Chloro-2-methylquinoline | HCID 77973 | — |
| Lösungsmittel | Glycol monoethyl ether | HCID 8076 | — |
| Produkt | 2-Methyl-4-(piperazin-1-yl)quinoline | HCID 702318 | 85% |
Reaktionsschritte
4-Chloro-2-methylquinoline (1.8 g, 10 mmol) and anhydrous piperazine (5.25 g, 60 mmol) were dissolved in ethyleneglycol monoethylether (15 ml) and stirred at 140° C. overnight. The mixture was concentrated under reduced pressure, toluene was added (2×100 ml) and the solvent removed under reduced pressure. To the residue was added 0.5 M NaOH (100 ml) and the mixture was extracted with a mixture of dichloromethane/diethylether/ethyl acetate (1:1:1, 3×100 ml). The combined organic phases were washed with brine, dried over sodium sulfate and the solvent was removed under reduced pressure. 2.78 g of an off-white solid (8.5 mmol, 85%) were obtained that were used directly in the next step.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08883791B2 |
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| Quelldatensatz | uspto-grants-2014_11 |
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| ORD ID | ord-c1581ae54b9d4b08ba0367fd12948db5 |
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| Quellennotiz | uspto-grants-2014_11 |
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