Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Ammonia | HCID 222 | — |
| Edukt | 2,6-Dichloro-3-(trifluoromethyl)pyridine | HCID 1810337 | — |
| Produkt | 6-Chloro-5-(trifluoromethyl)pyridin-2-amine | HCID 13064153 | 46% |
Reaktionsschritte
2,6-Dichloro-3-(trifluoromethyl)pyridine (5.00 g, 23.2 mmol) and 28% aqueous ammonia (150 mL) were placed in a 250 mL autoclave. The mixture was heated at 93° C. for 21 h. The reaction was cooled to rt and extracted with EtOAc (100 mL×3). The combined organic extracts were dried over anhydrous Na2SO4 and evaporated under vacuum to give the crude product, which was purified by column chromatography on silica gel (2-20% EtOAc in petroleum ether as eluant) to give 6-chloro-5-(trifluoromethyl)pyridin-2-amine (2.1 g, 46% yield). 1H NMR (400 MHz, DMSO-d6) δ 7.69 (d, J=8.4 Hz, 1H), 7.13 (br s, 2H), 6.43 (d, J=8.4 Hz, 1H). MS (ESI) m/z (M+H)+197.2
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08741933B2 |
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| Quelldatensatz | uspto-grants-2014_06 |
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| ORD ID | ord-278ad5d8ec7446beadfd5a43a5f4f93a |
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| Quellennotiz | uspto-grants-2014_06 |
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