Reaktion #3049

ord-f43f465340624f4daaa306b11664c6ec

Lösungsmittel

Reaktionsbedingungen

Temperatur
35°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturat reflux temperature for 50 hours
  2. 2
    Sonstigethe resulting layers were separated
  3. 3
    ExtraktionThe aqueous layer was extracted with 600 ml of diethyl ether
  4. 4
    Extraktionextract
  5. 5
    Trocknenthe resulting solution was dried over sodium sulfate overnight
  6. 6
    SonstigeAfter sodium sulfate removal
  7. 7
    Sonstigethe solvent was evaporated
  8. 8
    Sonstigeto provide

Vorschrift

Allyl bromide (69.2 ml), 2-t-butylphenol (122.9 ml) and potassium carbonate (121.6 g) were stirred in 265 ml of acetone at reflux temperature for 50 hours and then cooled to 35° C. Water (600 ml) was added and the resulting layers were separated. The aqueous layer was extracted with 600 ml of diethyl ether. The organic layer was combined with the aqueous layer's ether extract and the resulting solution was dried over sodium sulfate overnight. After sodium sulfate removal, the solvent was evaporated to provide, after further workup, 147 g of the subtitled intermediate.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05731336uspto-grants-1998_03