Reaktion #429556

ord-35267f997efc46afbb9e3be66cc9c2bc

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas refluxed for 3 hours
  2. 2
    Filtrationfiltered
  3. 3
    Sonstigeto remove the inorganic salts
  4. 4
    Sonstigeevaporated under vacuum
  5. 5
    workup.DISSOLUTIONThe crude product was dissolved in ether (100 mL)
  6. 6
    Waschenwashed with H2O (2×20 mL)
  7. 7
    TrocknenThe organic layer was dried (Na2SO4)
  8. 8
    Sonstigeevaporated
  9. 9
    Sonstigeto yield 4.5 g, 82.4% yield

Vorschrift

A mixture of 4'-hydroxy-3'-methylacetophenone (5.0 g, 33.3 mmol), iodomethane (5.7 g, 40.0 mmol), K2CO3 (granular, anhydrous) (23.0 g, 167 mmol), and acetone (250 mL) was refluxed for 3 hours. The reaction mixture was then cooled to room temperature, filtered to remove the inorganic salts, and evaporated under vacuum. The crude product was dissolved in ether (100 mL) and washed with H2O (2×20 mL). The organic layer was dried (Na2SO4) and evaporated to yield 4.5 g, 82.4% yield. The ketone was used in the following reaction without further purification.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05858684uspto-grants-1999_01