Reaktion #46030

ord-b88aec028ab3465a9637eaaccef53927

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.STIRRINGby stirring at ambient temperature for 4 hours
  2. 2
    SonstigeAfter terminating
  3. 3
    Sonstigethe reaction
  4. 4
    Extraktionthe aqueous layer was extracted with toluene, which
  5. 5
    workup.ADDITIONwas added to the organic layer
  6. 6
    Waschenthe organic layer was washed with a saturated salt solution
  7. 7
    Trocknendried over anhydrous magnesium sulfate
  8. 8
    workup.DISTILLATIONThe solvent was distilled off

Vorschrift

Under a nitrogen atmosphere, 1.52 g of sodium hydride was added to 9.45 g of 2-fluoro-3-((4-propylcyclohexyl)phenyl)phenol (5) dissolved in 60 mL of THF cooling with iced water, and the mixture was stirred at ambient temperature for 30 minutes. 3.07 g of chloromethyl methyl ether was added to the solution under cooling with iced water, followed by stirring at ambient temperature for 4 hours. After terminating the reaction by pouring water into the reaction solution, the aqueous layer was extracted with toluene, which was added to the organic layer, and the organic layer was washed with a saturated salt solution and then dried over anhydrous magnesium sulfate. The solvent was distilled off to obtain 11.6 g of 2-fluoro-3-((4-propylcyclohexyl)phenyl)-1-methoxymethoxybenzene (6).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07740769B2uspto-grants-2010_06