반응 #1933448

ord-03809669217847438386e987ffec98a4

용매

반응 조건

온도
116°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출The product was extracted with ethyl acetate
  2. 2
    세척washed with brine
  3. 3
    기타The solvent was evaporated in vacuo
  4. 4
    기타to leave a crude material which
  5. 5
    기타was purified by column chromatography (silica gel; 230-400 mesh; ethyl acetate/hexane=1:9)

실험 절차

To a solution of 7-fluoro-1H-benzo[d][1,3]oxazine-2,4-dione (1.00 g, 5.52 mmol) in anhydrous DMF (15 mL), 4-(sec-butyl)-aniline (B) (0.824 g, 5.52 mmol) was added and the reaction mixture was heated at 116° C. for 16 hours. The product was extracted with ethyl acetate and washed with brine. The solvent was evaporated in vacuo to leave a crude material which was purified by column chromatography (silica gel; 230-400 mesh; ethyl acetate/hexane=1:9) to give 2-amino-N-(4-sec-butyl-phenyl)-4-fluoro-benzamide (N) as white solid. Yield: 0.92 g (58%).

출처

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