تفاعل #1605813

ord-2d5602354ea84c34b8c1ca9d286ce53d

معادلة التفاعل

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

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةthe mixture was heated
  2. 2
    درجة الحرارةunder reflux overnight
  3. 3
    تركيزThe 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
    استخلاصfor extraction
  6. 6
    تجفيفThe organic layer was dried over sodium sulfate
  7. 7
    ترشيحafter filtration
  8. 8
    تركيزconcentrated under reduced pressure
  9. 9
    أخرىThe residue was purified by a silica gel column

الإجراء التجريبي

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).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09072734B2uspto-grants-2015_07