Potassium Carbonate → HCID 9921211, Verbindung

2-(1H-1,2,4-Triazol-3-yl)pyridine (0.24 g, 1.6 mmol), potassium carbonate (0.45 g, 3.2 mmol) and 3-fluorobenzonitrile (0.20 g, 1.6 mmol) were stirred in DMF (20 mL) at ambient temperature. The resulting reaction mixture was heated at 145° C. for 16 h, after which time it was quenched with H2O (30 mL) and diluted with EtOAc (200 mL). The EtOAc solution was washed with H2O (3×100 mL), then brine (100 mL) and dried (MgSO4), filtered, and concentrated in vacuo. The resulting residue was chromatographed on silica gel eluting with hexane:EtOAc (40:60) to afford 3-(3-pyridin-2-yl-1H-1,2,4-triazol-1-yl)benzonitrile as a white solid.

1. customThe resulting reaction mixture
2. customafter which time it was quenched with H2O (30 mL)
3. additiondiluted with EtOAc (200 mL)
4. washThe EtOAc solution was washed with H2O (3×100 mL)
5. dry with materialbrine (100 mL) and dried (MgSO4)
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. customThe resulting residue was chromatographed on silica gel eluting with hexane:EtOAc (40:60)

ORD-Eintrag

ord-9ad3c0d5134a412b8df25da103bfbd1c

Quelldatensatz

uspto-grants-2006_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07105548B2