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

HRID 59936

반응식

HRID 59936 반응식
[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]

참가 물질

5

반응물 2

HCID 807IodineHCID 27564314-Amino-3-fluorobenzonitrile

생성물 1

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

시약·촉매·용매 2

HCID 159865Silver sulfate촉매HCID 702Ethanol용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-0440163263d74d16a1464a8da506aac9
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09440929B2

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