1-Bromo-3-iodo-5-nitrobenzene → 3-Bromo-5-iodoaniline

HRID 446996

반응식

HRID 446996 반응식
[Br:1][C:2]1[CH:3]=[C:4]([N+:9]([O-])=O)[CH:5]=[C:6]([I:8])[CH:7]=1>C(O)(=O)C.C(OCC)(=O)C.[Fe]>[Br:1][C:2]1[CH:3]=[C:4]([CH:5]=[C:6]([I:8])[CH:7]=1)[NH2:9]

참가 물질

5

반응물 1

HCID 454803871-Bromo-3-iodo-5-nitrobenzene

생성물 1

HCID 454803883-Bromo-5-iodoaniline수율 96.2%

시약·촉매·용매 3

HCID 23925Iron촉매HCID 176Acetic Acid용매HCID 8857Ethyl Acetate용매

실험 절차

A mixture of 3-Bromo-5-iodonitrobenzene (4.21 g, 0.0128 mol) and iron powder (3.6 g, 0.0642 mol) in glacial acetic acid (50 ml) was stirred at ambient temperature for 16 h. The reaction mixture was then filtered through a pad of celite and washed through with ethyl acetate. The filtrate was evaporated in vacuo to give a brown oil. This was re-dissolved in ethyl acetate, loaded onto a large pad of silica and eluted with ethyl acetate. The filtrate was evaporated in vacuo to afford 3-Bromo-5-iodoaniline as a brown solid (3.67 g, 96%) which was used without further purification.

후처리

  1. filtrationThe reaction mixture was then filtered through a pad of celite
  2. washwashed through with ethyl acetate
  3. customThe filtrate was evaporated in vacuo
  4. customto give a brown oil
  5. washeluted with ethyl acetate
  6. customThe filtrate was evaporated in vacuo

출처 및 근거

ORD 기록
ord-94195ee6de80480dad563653fe5d2f25
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08481544B2

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