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

HRID 446996

反応式

HRID 446996 の反応式
[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]

参加物

5

反応物 1

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

生成物 1

HCID 454803883-Bromo-5-iodoaniline収率 96.2%

試薬・触媒・溶媒 3

HCID 23925Iron触媒HCID 176Acetic Acid溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-94195ee6de80480dad563653fe5d2f25
出典データセット
uspto-grants-2013_07
特許番号
US08481544B2

関連ノート

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