تفاعل #88214

معادلة التفاعل

4-amino-3-fluorobenzonitrile

I2

→

desired product

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

المذيبات

EtOH

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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.

المصدر