Reaktion #560806

ord-982a471bee604723b4b7c88e00e160e7

Lösungsmittel

Reaktionsbedingungen

Temperatur
95°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturAfter cooling to room temperature
  2. 2
    Extraktionextracted with CH2Cl2 (3×)
  3. 3
    TrocknenThe combined organics were dried over Na2SO4
  4. 4
    Filtrationfiltered
  5. 5
    Einengenconcentrated
  6. 6
    SonstigeThe residue was purified

Vorschrift

A mixture of 2-fluoropyridin-3-ylboronic acid (0.748 g, 5.3 mmol), 4-bromo-2-(trifluoromethyl)pyridine (1.00 g, 4.4 mmol), Pd(PPh3)2Cl2 (0.155 g, 0.22 mmol) and sodium carbonate (0.797 g, 13.3 mmol) in DME (6.5 mL), ethanol (1.9 mL) and water (0.47 mL) was heated to 95° C. for 2 h. After cooling to room temperature, the mixture was diluted with H2O and extracted with CH2Cl2 (3×). The combined organics were dried over Na2SO4, filtered and concentrated. The residue was purified using column chromatography (EtOAc/Hexanes=0→20%) to give the title compound. MS (ESI, pos. ion) m/z: 243 (M+1).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08637500B2uspto-grants-2014_01