Reaktion #160530

ord-d6372bf02a004b0890cfcdbe6e270fb0

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionthis mixture was extracted with ethyl acetate
  2. 2
    WaschenThis organic layer was washed with water and brine
  3. 3
    Trocknendried over anhydrous magnesium sulfate
  4. 4
    SonstigeThe solvent was removed under reduced pressure
  5. 5
    SonstigeThe residue was purified by column chromatography on silica gel (eluent: n-hexane/ethyl acetate)

Vorschrift

To a solution of dimethyl-(4-nitro-2-trifluoromethylphenyl)amine (0.95 g) in N,N-dimethylformamide (20 mL) were added (4-chlorophenoxy)acetonitrile (0.75 g) and 1 mol/L potassium tert-butoxide (4.5 mL, in tetrahydrofuran solution) under ice cooling, and this mixture was stirred at the same temperature for 1 hour. This reaction mixture was poured into water, and this mixture was extracted with ethyl acetate. This organic layer was washed with water and brine, and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure. The residue was purified by column chromatography on silica gel (eluent: n-hexane/ethyl acetate) to give the title compound (0.11 g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08829040B2uspto-grants-2014_09