반응 #1933457

ord-4df33a92f03240109a1b97594008ec40

반응 조건

온도
80°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타the solvent was removed under reduced pressure
  2. 2
    workup.ADDITIONthe residue was diluted with ethyl acetate
  3. 3
    세척washed with 1 N aqueous solution of sodium hydroxide, water
  4. 4
    건조dried over sodium sulfate
  5. 5
    기타The crude oil (7 g) was purified by column chromatography (silica gel 230-400 mesh; 10/0 to 4/1 hexanes/EtOAc as eluent)

실험 절차

To a solution of isatoic anhydride (4.00 g, 24.0 mmol) in N,N-dimethyl formamide (80 mL) under nitrogen atmosphere was added 4-sec-butylaniline (3.66 g, 24.0 mmol). The reaction mixture was heated at 80° C. for 24 hours, then the solvent was removed under reduced pressure and the residue was diluted with ethyl acetate, washed with 1 N aqueous solution of sodium hydroxide, water, and dried over sodium sulfate. The crude oil (7 g) was purified by column chromatography (silica gel 230-400 mesh; 10/0 to 4/1 hexanes/EtOAc as eluent) to give pure 2-amino-N-(4-sec-butylphenyl)-benzamide as a brown solid. Yield: 1.8 g (27.3%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08952021B2uspto-grants-2015_02