HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Acetonitrile → 2-Fluoro-5-nitropyridine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Acetonitrile | HCID 6342 | — |
| Edukt | 2-Chloro-5-nitropyridine | HCID 78308 | — |
| Edukt | Potassium Fluoride | HCID 522689 | — |
| Katalysator | Tetraphenylphosphonium Bromide | HCID 2724163 | — |
| Lösungsmittel | Diethyl Ether | HCID 3283 | — |
| Produkt | 2-Fluoro-5-nitropyridine | HCID 95264 | — |
Reaktionsschritte
2-Chloro-5-nitropyridine (100 g, 0.656 mol, Aldrich), KF (84.1 g, 1.448 mol), Ph4PBr (95.3 g, 0.227 mol) and acetonitrile (1.5 L) were combined and heated at reflux until no starting material remained. The volume was reduced to 750 mL, and the mixture was diluted with 2 L of ether, filtered and concentrated. The residue was triturated with hot hexane (5×1 L). The hexane extracts were combined and concentrated to afford 48 g (54%). 1H NMR (CDCl3, 300 MHz) δ7.15 (dd, J=3, 6 Hz, 1H), 8.64 (m, 1H), 9.15 (d, J=1.6 Hz, 1H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05733912 |
| Quelldatensatz | uspto-grants-1998_03 |
| ORD ID | ord-c3b0e2987bf6463288457f21739f34ea |
| Quellennotiz | uspto-grants-1998_03 |