Reaktion #167126

ord-c9722d991b724d028bda6863424319d1

Lösungsmittel

Reaktionsbedingungen

Temperatur
150°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Filtrationthe mixture was filtered
  2. 2
    Sonstigeevaporated under vacuum
  3. 3
    workup.ADDITIONThe fractions containing product
  4. 4
    Sonstigethe solvent was removed under reduced pressure

Vorschrift

2-Bromo-3,5-dimethoxy-benzoic acid methyl ester (5.2 g) was dissolved in DMF (16 mL), and Cu powder (2.4 g) was added. After stirring at 150° C. for 3 days, the mixture was filtered and evaporated under vacuum. The crude material was subjected to silica gel chromatography using effluent of 30-60% ethyl acetate and hexanes. The fractions containing product were combined and the solvent was removed under reduced pressure to provide 4,6,4′,6′-tetramethoxy-biphenyl-2,2′-dicarboxylic acid dimethyl ester (2.5 g, 68%) as a clear oil.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08841278B2uspto-grants-2014_09