Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | 1-Methylpiperazine | HCID 53167 | — |
| Edukt | 6-(4-chloro-2-pyridinyl)-2-pyridin-2-yl-1H-pyrimidin-4-one | HCID 178515630 | — |
| Katalysator | Zincchloride | HCID 3007855 | — |
| Lösungsmittel | 2-Methyl-2-butanol | HCID 6405 | — |
| Produkt | HCID 178480770 | HCID 178480770 | — |
Reaktionsschritte
A mixture of 3.51 g (12.3 mmol) of 6-(4-chloropyrid-2-yl)-2-pyrid-2-yl-pyrimidin-4-ol, 27.4 ml (303 mmol, 20 equivalents, 30.38 g) of 1-methyl-piperazine and 84 mg (0.05 mmol, 0.05 equivalent) of zinc(II) chloride in 50 ml of 2-methyl-2-butanol is refluxed for 22 hours and concentrated to dryness using a rotary evaporator. 50 ml of water are added, 3.6 g of EDTA are added, and the pH is adjusted to 9 using dilute sodium hydroxide solution. Extraction is carried out three times using 150 ml of chloroform each time, and the organic extracts are combined and dried (sodium sulfate). Concentration is carried out using a rotary evaporator and the crude product is recrystallised from toluene. 6-[4-(4-Methyl-piperazin-1-yl)-pyrid-2-yl]-2-pyrid-2-yl-pyrimidin-4-ol is obtained in the form of a whitish solid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US07138363B2 |
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| Quelldatensatz | uspto-grants-2006_11 |
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| ORD ID | ord-62dccb50952a4f20b9d581bd7a6a4f81 |
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| Quellennotiz | uspto-grants-2006_11 |
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