Iodine → 4-Amino-3-fluoro-5-iodobenzonitrile
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
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
- filtrationThe mixture was filtered
- concentrationconcentrated
- dissolutionThe residue was dissolved in EtOAc
- washwashed (sat. Na2S2O3×3)
- dry with materialThe organic layer was dried (Na2SO4)
- concentrationconcentrated
- 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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