Reaktion #70300

ord-a11cea2e8f2340d298289a02033d0720

Lösungsmittel

Reaktionsbedingungen

Temperatur
130°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe solvent was evaporated
  2. 2
    Extraktionthe crude mixture was extracted between water and ethyl acetate
  3. 3
    SonstigeThe solid residue was purified by chromatography over SiO2 eluting with DCM/methanol

Vorschrift

In a schlenck tube, a mixture of 2,5-dibromopyridine (2.11 mmol, 0.500 g), 3-fluoro-4-(tributylstannyl)pyridine (2.32 mmol, 0.896 g), PdCl2(PPh3)2 (0.21 mmol, 0.148 g), CuI (0.43 mmol, 0.080 g) in DMF (5 ml) was heated at 130° C. for 12 hours, under argon atmosphere. The solvent was evaporated and the crude mixture was extracted between water and ethyl acetate. The solid residue was purified by chromatography over SiO2 eluting with DCM/methanol mixtures affording 0.330 g (yield 62%) of the expected product.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08536165B2uspto-grants-2013_09