Reaktion #2335938

ord-c037378908494ffbbffa2ae2d5695fcf

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturis cooled in an ice bath
  2. 2
    Extraktionthe mixture is extracted with methylene chloride
  3. 3
    TrocknenThe organic layer is dried over anhydrous sodium sulfate
  4. 4
    workup.DISTILLATIONthe solvent is distilled off under reduced pressure
  5. 5
    SonstigeThe resulting crude crystals are recrystallized from ethanol

Vorschrift

To a solution of 2-amino-6-(ethylamino)benzonitrile (2.3 g) in methylene chloride (50 ml) is added pyridine (1.6 ml), and thereto is added dropwise propionyloxyacetyl chloride (3.0 ml) which is cooled in an ice bath. The mixture is stirred at room temperature for 1 hour, and thereafter, water is added thereto, and the mixture is extracted with methylene chloride. The organic layer is dried over anhydrous sodium sulfate, and the solvent is distilled off under reduced pressure. The resulting crude crystals are recrystallized from ethanol to give the title compound (1.6 g) having the following physical properties.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05041462uspto-grants-1991_08