반응 #88083

ord-9459193e86ed4825aac16c791697ebcc

반응 조건

온도
70°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도cooled to room temperature
  2. 2
    기타partitioned between ethyl acetate
  3. 3
    기타The organic layer was separated
  4. 4
    건조dried over MgSO4
  5. 5
    여과filtered
  6. 6
    농축concentrated under reduced pressure

실험 절차

To a solution of 4-amino-3-iodo-5-nitro-benzoic acid methyl ester in ethyl acetate (50 mL) was added SnCl2 dihydrate. The mixture was heated to 70° C. for two hours, then cooled to room temperature and partitioned between ethyl acetate and satruated aqueous sodium bicarbonate. The organic layer was separated, dried over MgSO4, filtered and concentrated under reduced pressure to provide 1.68 g (quantitative) of 3,4-diamino-5-iodo-benzoic acid methyl ester.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09440956B2uspto-grants-2016_09