反応 #88214

反応方程式

4-amino-3-fluorobenzonitrile

I2

→

desired product

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

溶媒

EtOH

反応条件

後処理

1. 1
   ろ過The mixture was filtered
2. 2
   濃縮concentrated
3. 3
   workup.DISSOLUTIONThe residue was dissolved in EtOAc
4. 4
   洗浄washed (sat. Na2S2O3×3)
5. 5
   乾燥The organic layer was dried (Na2SO4)
6. 6
   濃縮concentrated
7. 7
   その他The residue was purified by flash column chromatography (SiO2, 95:5 to 70:30 cyclohexane/EtOAc)

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.

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