반응 #49274

ord-7387e8246d2a488ebc482fbdeadd6168

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출extracted with ethyl acetate
  2. 2
    세척The organic layer was washed with 0.5 mol/L hydrochloric acid and saturated brine
  3. 3
    건조dried over anhydrous sodium sulfate
  4. 4
    기타The solvent was evaporated under reduced pressure
  5. 5
    기타the residue was purified by slurry

실험 절차

Iodine (6.29 g, 24.8 mmol) was dissolved in ethanol (225 mL), and the solution was added with silver sulfate (3.87 g, 12.4 mmol) and 3-amino-6-bromophthalimide (3.00 g, 12.4 mmol), followed by stirring at room temperature for 23 hours. The reaction mixture was added with 10% aqueous sodium thiosulfate solution and extracted with ethyl acetate. The organic layer was washed with 0.5 mol/L hydrochloric acid and saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, the residue was purified by slurry using hexane and methanol to obtain 3-amino-4-iodo-6-bromophthalimide (4.3 g. yield 96%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07745641B2uspto-grants-2010_06