Iodine → 4-Amino-3-fluoro-5-iodobenzonitrile

HRID 59936

反応式

HRID 59936 の反応式
[NH2:1][C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[CH:4][C:3]=1[F:10].[I:11]I>CCO.[O-]S([O-])(=O)=O.[Ag+].[Ag+]>[NH2:1][C:2]1[C:9]([I:11])=[CH:8][C:5]([C:6]#[N:7])=[CH:4][C:3]=1[F:10]

参加物

5

反応物 2

HCID 807IodineHCID 27564314-Amino-3-fluorobenzonitrile

生成物 1

HCID 442031204-Amino-3-fluoro-5-iodobenzonitrile

試薬・触媒・溶媒 2

HCID 159865Silver sulfate触媒HCID 702Ethanol溶媒

実験手順

A mixture of 4-amino-3-fluorobenzonitrile (147 mmol), I2 (147 mmol) and Ag2SO4 (147 mmol) in EtOH (700 mL) was stirred at room temperature for 1.5 h. The mixture was filtered and concentrated. The residue was dissolved in EtOAc and washed (sat. Na2S2O3×3). The organic layer was dried (Na2SO4) and concentrated. The residue was purified by flash column chromatography (SiO2, 95:5 to 70:30 cyclohexane/EtOAc) to yield the desired product.

後処理

  1. filtrationThe mixture was filtered
  2. concentrationconcentrated
  3. dissolutionThe residue was dissolved in EtOAc
  4. washwashed (sat. Na2S2O3×3)
  5. dry with materialThe organic layer was dried (Na2SO4)
  6. concentrationconcentrated
  7. customThe residue was purified by flash column chromatography (SiO2, 95:5 to 70:30 cyclohexane/EtOAc)

出典と根拠

ORDレコード
ord-0440163263d74d16a1464a8da506aac9
出典データセット
uspto-grants-2016_09
特許番号
US09440929B2

関連ノート

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