HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triphenylphosphine → 3-Cyano-2-fluoropyridine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triphenylphosphine | HCID 11776 | — |
| Edukt | 2-Fluoronicotinamide | HCID 252367 | — |
| Lösungsmittel | Carbon Tetrachloride | HCID 5943 | — |
| Lösungsmittel | 1,1-Dichloroethane | HCID 6365 | — |
| Produkt | 3-Cyano-2-fluoropyridine | HCID 2783254 | 64,8% |
Reaktionsschritte
Add resin bound triphenylphosphine (4.0 g, 12.0 mmol) to a solution of 2-fluoro-nicotinamide (0.6 g, 4.3 mmol) in dichloroethane (20.0 mL) and carbon tetrachloride (20.0 mL). Reflux for 18 hours, cool to RT, filter, and concentrate the filtrate under vacuum. Purify by flash column on silica gel eluting with 10-60% EtOAc in hexanes to give the title compound (0.34 g, 64%). MS (ES) 123.1 (M+1)+. 1H NMR (400 MHz, CHCl3) δ 8.46 (m, 1H), 8.09 (m, 1H), 7.37 (m, 1H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07595339B2 |
| Quelldatensatz | uspto-grants-2009_09 |
| ORD ID | ord-f785c08da873469b9a460065bb3c21ab |
| Quellennotiz | uspto-grants-2009_09 |