Reaktion #157917

ord-18532b48adef474fa62a79baa547041c

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe reaction temperature was raised to room temperature after 1 h
  2. 2
    workup.STIRRINGStirred 2 h
  3. 3
    Extraktionaqueous phase was extracted dichloromethane (2×30 mL)
  4. 4
    EinengenThe combined organic phase was concentrated
  5. 5
    Sonstigepurified by flash chromatography (eluent: dichloromethane)

Vorschrift

NaH (60% in mineral oil, 1.2 g, 30 mmol) was added to an ice-cooled solution of (4-hydroxy-phenyl)-phenyl-methanone (5 g, 25.2 mmol) in DMF (25 mL). Stirred for 20 minutes at room temperature. Benzyl bromide (6.1 ml, 50 mmol) was added at 0° C. The reaction temperature was raised to room temperature after 1 h. Stirred 2 h. Water (20 mL) was added and aqueous phase was extracted dichloromethane (2×30 mL). The combined organic phase was concentrated and purified by flash chromatography (eluent: dichloromethane). 1H nmr revealed the product was pure. Yield: 7.0 g, 96%

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08822548B2uspto-grants-2014_09