반응 #160529

ord-34e2102f3be048bb8fdf402940869913

반응 조건

온도
50°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

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

실험 절차

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).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08829040B2uspto-grants-2014_09