Reaktion #66964

ord-e673fc95c5dc498dbd7b380bc5559795

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe mixture was cooled to 0° C.
  2. 2
    Sonstigequenched with saturated aqueous NaHCO3
  3. 3
    Extraktionextracted with EtOAc
  4. 4
    TrocknenThe combined organic layers were dried over MgSO4
  5. 5
    Filtrationfiltered
  6. 6
    Einengenconcentrated
  7. 7
    Sonstigethe residue was purified by silica gel chromatography

Vorschrift

To (2′-hydroxymethyl-6-methoxy-4′-trifluoromethyl-biphenyl-3-yl)-acetic acid ethyl ester (2.30 mmol) in DME was added phosphorus tribromide (0.26 mL, 2.76 mmol), and the reaction was stirred for 3 hours at room temperature. The mixture was cooled to 0° C., quenched with saturated aqueous NaHCO3, and extracted with EtOAc. The combined organic layers were dried over MgSO4, filtered, and concentrated, and the residue was purified by silica gel chromatography to give the title compound.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08524748B2uspto-grants-2013_09