Reaktion #423779

ord-13de4e6d8e0344ba87e154010480c2a1

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthe solution was heated to 130° C. for 1 hour
  2. 2
    TemperaturThe solution was cooled
  3. 3
    Waschenwashed with 1 M aqueous HCl three times
  4. 4
    Waschenwashed with brine
  5. 5
    Trocknendried over anhydrous sodium sulfate
  6. 6
    FiltrationAfter filtration
  7. 7
    Sonstigethe solvent was removed under vacuum

Vorschrift

1-Adamantanethiol (278 mg) was dissolved in dimethyl sulfoxide (10 mL). Sodium hydride (60% in mineral oil, 42 mg) was added, and the solution was stirred at room temperature for 20 minutes. 2-Bromo-6-fluorobenzonitrile (300 mg) was added and the solution was heated to 130° C. for 1 hour. The solution was cooled, added to diethyl ether, washed with 1 M aqueous HCl three times, washed with brine, and dried over anhydrous sodium sulfate. After filtration, the solvent was removed under vacuum to yield the title compound.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08889675B2uspto-grants-2014_11