Reaktion #160529

ord-34e2102f3be048bb8fdf402940869913

Lösungsmittel

Reaktionsbedingungen

Temperatur
50°CELSIUS
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 1-floro-4-nitro-2-trifluoromethylbenzene (2.0 g) in tetrahydrofuran (20 mL) were added dimethyamine (0.64 g) and sodium hydride (0.34 g) at room temperature, and this mixture was stirred at 50° C. for 16 hours. 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 (0.94 g).

Quelle

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