Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Ammonia | HCID 222 | — |
| Edukt | 1-(5-Bromo-3-fluoro-2-nitro-phenyl)-1H-pyrazole | HCID 67004648 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Produkt | HCID 67004761 | HCID 67004761 | 86% |
Reaktionsschritte
To a solution of 1-(5-bromo-3-fluoro-2-nitro-phenyl)-1H-pyrazole (240 mg, 0.84 mmol) in ethanol (3 mL) was added ammonia (3 mL, 2N in methanol. The resulting mixture was heated in a sealed tube at 80° C. for 16 hours then concentrated in vacuo. The residue was purified by column chromatography over silica gel eluted with ethyl acetate:hexanes (1:3) to afford 205 mg (86%) of the title compound as a yellow solid. 1H NMR (CDCl3) δ 5.20 (br s, 2H), 6.50 (t, 1H), 6.9 (d, 1H), 7.1 (d, 1H), 7.7 (d, 1H), 7.8 (d, 1H). MS M+1 283, M+1+2 285.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US07582641B2 |
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| Quelldatensatz | uspto-grants-2009_09 |
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| ORD ID | ord-05fa6e6ee62b481080310edc38c731e5 |
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| Quellennotiz | uspto-grants-2009_09 |
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