Reaktion #45927

ord-0b8aca2fd88841b99fc0aa3fcbd77d96

Lösungsmittel

Reaktionsbedingungen

Temperatur
90°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas heated
  2. 2
    SonstigeThe reaction was quenched by cold H2O (50 mL)
  3. 3
    Extraktionthe resulting mixture was extracted with EtOAc (3×100 mL)
  4. 4
    WaschenThe combined EtOAc extracts were washed with brine (2×50 mL)
  5. 5
    Trocknendried (anhydrous Na2SO4)
  6. 6
    SonstigeThe solvent was removed in vacuo
  7. 7
    Sonstigethe crude products were purified by silica gel column chromatography (eluting with 10% EtOAc in hexane)

Vorschrift

A mixture of 2-n-butylamino-4-fluoronitrobenzene (10 mmol), 4-t-butylphenol (13 mmol), solid K2CO3 (30 mmol) and DMF (30 mL) was heated with stirring at 90° C. for 10 h. The reaction was quenched by cold H2O (50 mL), and the resulting mixture was extracted with EtOAc (3×100 mL). The combined EtOAc extracts were washed with brine (2×50 mL) and dried (anhydrous Na2SO4). The solvent was removed in vacuo, and the crude products were purified by silica gel column chromatography (eluting with 10% EtOAc in hexane), giving 2-n-butylamino-4-(4-t-butylphenoxy)nitrobenzene.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07737285B2uspto-grants-2010_06