Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Ethyl Acetate | HCID 8857 | — |
| Edukt | 1,1'-Biphenyl, mixt. with 1,1'-oxybis(benzene) | HCID 24670 | — |
| Edukt | 5-((5-Fluoropyridin-3-ylamino)methylene)-2,2-dimethyl-1,3-dioxane-4,6-dione | HCID 67503407 | — |
| Lösungsmittel | Diethyl Ether | HCID 3283 | — |
| Produkt | HCID 178516441 | HCID 178516441 | — |
Reaktionsschritte
To a stirred solution of Dowtherm A at 250° C., was added 5-(((5-fluoropyridin-3-yl)amino)methylene)-2,2-dimethyl-1,3-dioxane-4,6-dione (1 g, 0.003 mol) portionwise over a period of 10 minutes. The reaction was monitored by TLC (TLC eluent: 50% EtOAc in petroleum ether, uv active). After completion of reaction, the mixture was cooled to ambient temperature and treated with diethyl ether to obtain a grey precipitate. The precipitate was stirred for 5-10 minutes and filtered, washed with diethyl ether and dried under vacuum to obtain 7-fluoro-1,5-naphthyridin-4-ol as a tan colored solid, (0.4 g, 64.93%). 1H NMR (400 MHz, DMSO-d6): δ 12.68 (bs, 1H), 9.43 (s, 1H), 8.75 (t, J=6.4 Hz, 1H), 8.59 (d, J=8, 1H), 6.99 (d, J=17.2 Hz, 1H). m/z (ESI) 165.1 (M+H)+.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US09340549B2 |
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| Quelldatensatz | uspto-grants-2016_05 |
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| ORD ID | ord-f0faf7c99d694e7783d7fcc6c66610ef |
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| Quellennotiz | uspto-grants-2016_05 |
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