Reaktion #47077

ord-e4fef959462742fb85a879cdd12a04bb

Lösungsmittel

Reaktionsbedingungen

Temperatur
50°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe reaction mixture is cooled to RT
  2. 2
    Waschenwashed with water, brine
  3. 3
    Trocknendried (MgSO4)
  4. 4
    Filtrationfiltered
  5. 5
    SonstigeThe filtrate is evaporated
  6. 6
    Sonstigethe residue purified by chromatography on silica gel
  7. 7
    Waschenelution with dichloromethane

Vorschrift

To a solution of 2-fluorophenol (560 mg, 5.0 mmol) in DMF (10 mL) is added potassium carbonate (828 mg, 6.0 mmol) followed by chloroacetonitrile (0.315 mL, 50.0 mmol). The reaction mixture is stirred and heated at 50° C. for 14 h. The reaction mixture is cooled to RT, diluted with EtOAc, and washed with water, brine, then dried (MgSO4), and filtered. The filtrate is evaporated, and the residue purified by chromatography on silica gel; elution with dichloromethane gives 736 mg of the product 384.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07741493B2uspto-grants-2010_06