반응 #88214

반응 방정식

4-amino-3-fluorobenzonitrile

I2

→

desired product

4-Amino-3-fluoro-5-iodo-benzonitrile

용매

EtOH

반응 조건

후처리

1. 1
   여과The mixture was filtered
2. 2
   농축concentrated
3. 3
   workup.DISSOLUTIONThe residue was dissolved in EtOAc
4. 4
   세척washed (sat. Na2S2O3×3)
5. 5
   건조The organic layer was dried (Na2SO4)
6. 6
   농축concentrated
7. 7
   기타The residue was purified by flash column chromatography (SiO2, 95:5 to 70:30 cyclohexane/EtOAc)

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.

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