Iodine → 5-Ethyl-2-iodophenol

HRID 1167307

反応式

HRID 1167307 の反応式
[I:1]I.[CH2:3]([C:5]1[CH:6]=[C:7]([OH:11])[CH:8]=[CH:9][CH:10]=1)[CH3:4].C([O-])(=O)C.[Tl+]>C(Cl)Cl>[CH2:3]([C:5]1[CH:10]=[CH:9][C:8]([I:1])=[C:7]([OH:11])[CH:6]=1)[CH3:4]

参加物

5

反応物 3

HCID 807IodineHCID 11247thallium(I) acetateHCID 121013-Ethylphenol

生成物 1

HCID 229961995-Ethyl-2-iodophenol収率 56.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

Iodine (6.35 g, 25 mmol) in methylene chloride (360 mL) was added dropwise over 3 h to a stirred suspension of 3-ethyl-phenol (3.05 g, 25 mmol) and thallium (I) acetate (7.90 g, 30 mmol) in methylene chloride (300 mL). The resulting mixture was stirred at room temperature for 24 h and filtered. The filtrate was concentrated in vacuo and the residue was purified by flash chromatography (Biotage system, KP-Sil™ 32-63 μm, 60 Å silica gel) eluting with 0-5% ethyl acetate in hexanes to afford 5-ethyl-2-iodophenol (3.49g, 56%).

後処理

  1. filtrationfiltered
  2. concentrationThe filtrate was concentrated in vacuo
  3. customthe residue was purified by flash chromatography (Biotage system, KP-Sil™ 32-63 μm, 60 Å silica gel)
  4. washeluting with 0-5% ethyl acetate in hexanes

出典と根拠

ORDレコード
ord-d91fbeefaf3d4c6fb2787296c9dca273
出典データセット
uspto-grants-2003_09
特許番号
US06617346B1

関連ノート

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