Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Ammonia | HCID 222 | — |
| Edukt | 2-Bromo-5-fluoro-3-nitropyridine | HCID 20791243 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Produkt | 5-Fluoro-3-nitropyridin-2-amine | HCID 21717339 | 67% |
Reaktionsschritte
A solution of 2-bromo-5-fluoro-3-nitropyridine (1.176 g, 5.321 mmol) in 2M NH3 in MeOH (20 ml) was sealed in an autoclave and then heated at 75° C. for 6 h and then at 90° C. for a further 18 h. The reaction mixture was then cooled and evaporated, treated with sat. aq. NaHCO3 (100 ml) and then extracted with 5% MeOH/DCM (3×200 ml). The combined organic phases were dried and the solvent was removed. The residue was subjected to column chromatography on silica gel using a 0-5% MeOH in DCM gradient to provide the desired compound as a yellow solid (561 mg, 67%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08071592B2 |
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| Quelldatensatz | uspto-grants-2011_12 |
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| ORD ID | ord-1b5765252d184358ababd3851fe7a8f5 |
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| Quellennotiz | uspto-grants-2011_12 |
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