Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Pyridine | HCID 1049 | — |
| Edukt | Isonicotinic Acid | HCID 5922 | — |
| Edukt | 1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide | HCID 15908 | — |
| Edukt | 3-Amino-5-(trifluoromethyl)-1,2-dihydropyridin-2-one | HCID 2315787 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | HCID 178522158 | HCID 178522158 | 76,9% |
Reaktionsschritte
A mixture of 1.0 g of 3-amino-2-hydroxy-5-trifluoromethylpyridine, 0.69 g of isonicotinic acid, 1.40 g of WSC and 7 ml of pyridine was stirred while heating at 80° C. for two hours. The reaction mixture was cooled to room temperature, and then water was added to the reaction mixture, followed by extraction with ethyl acetate three times. The combined organic layers were washed with water and a saturated sodium chloride solution, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to give 1.22 g of N-[2-hydroxy-5-(trifluoromethyl)pyridin-3-yl]isonicotinamide.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08609705B2 |
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| Quelldatensatz | uspto-grants-2013_12 |
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| ORD ID | ord-500b2b4684cd4307aae19747844ee53d |
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| Quellennotiz | uspto-grants-2013_12 |
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