Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Sodium Nitrite | HCID 23668193 | — |
| Edukt | 2-amino-6-fluoro-benzoic acid N'-(2-fluoro-phenyl)-hydrazide | HCID 68528398 | — |
| Lösungsmittel | Hydrochloric Acid | HCID 313 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Water ethanol | HCID 19096565 | — |
| Produkt | HCID 178518865 | HCID 178518865 | 95% |
Reaktionsschritte
Intermediate 44 (2.182 g, 8.289 mmol) was suspended in 1M HCl (20 ml), cooled to 0° C. and treated dropwise with a solution of sodium nitrite (1.144 g, 16.58 mmol) in water (7 ml). The mixture was stirred for 10 minutes at 0° C., diluted with 1:1 EtOH/H2O (30 ml) and heated to reflux for 3 hours, then stirred at room temperature for 18 hours. The solid was filtered, rinsed with water and dried to afford 1.939 g (95%) of 4-fluoro-1-(2-fluoro-phenyl)-1H-indazol-3-ol (Intermediate 45) as a tan solid. MS (APCI): (M+1)=247.1, (M−1)=245.0.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US07423054B2 |
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| Quelldatensatz | uspto-grants-2008_09 |
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| ORD ID | ord-42ec122c690144d88b4a34901f72d5a9 |
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| Quellennotiz | uspto-grants-2008_09 |
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