Reaktion #44453

ord-efae84e757614749b3b88bf9a2fe4d09

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe resulting mixture was heated
  2. 2
    Temperaturto reflux
  3. 3
    workup.STIRRINGstirred overnight
  4. 4
    Temperaturat reflux
  5. 5
    Extraktionfollowed by extraction with ethyl acetate (3×)
  6. 6
    WaschenThe combined organic layers were washed with water and brine
  7. 7
    Trocknendried (Na2SO4)
  8. 8
    Sonstigeevaporated

Vorschrift

Cs2CO3 (4 g, 12.3 mmol) was added to a solution of phenol (1 g, 10.6 mmol) in 50 mL of THF under N2 atmosphere. After stirring for 15 min. 1,4-dibromo-2-nitrobenzene (2.81 g, 10 mmol) was added. The resulting mixture was heated to reflux and stirred overnight at reflux. Water and ethyl acetate were added, followed by extraction with ethyl acetate (3×). The combined organic layers were washed with water and brine, dried (Na2SO4) and evaporated to give the crude compound (3.2 g, 75%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07737136B2uspto-grants-2010_06