반응 #1605813

ord-2d5602354ea84c34b8c1ca9d286ce53d

반응 방정식

CC(=O)Nc1ccc(Br)cc1-c1ccccc1
2-Phenyl-4-bromo-N-acetylaniline
Cl
hydrochloric acid
Nc1ccc(Br)cc1-c1ccccc1
2-phenyl-4-bromoaniline
수율 98.8%

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도the mixture was heated
  2. 2
    온도under reflux overnight
  3. 3
    농축The solution was concentrated under reduced pressure and to the residue
  4. 4
    workup.ADDITIONwere added ethyl acetate (50 mL) and water (40 mL)
  5. 5
    추출for extraction
  6. 6
    건조The organic layer was dried over sodium sulfate
  7. 7
    여과after filtration
  8. 8
    농축concentrated under reduced pressure
  9. 9
    기타The residue was purified by a silica gel column

실험 절차

2-Phenyl-4-bromo-N-acetylaniline (7.79 g, 26.85 mmol) was dissolved in ethanol (100 mL), 2 N hydrochloric acid (33.56 mmol, 67.12 mL) was added dropwise under ice bath, and the mixture was heated under reflux overnight. The solution was concentrated under reduced pressure and to the residue were added ethyl acetate (50 mL) and water (40 mL) for extraction. The organic layer was dried over sodium sulfate and, after filtration, concentrated under reduced pressure. The residue was purified by a silica gel column to obtain 2-phenyl-4-bromoaniline (6.58 g).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09072734B2uspto-grants-2015_07