反应详情

温度

160 °C

A mixture of 4-iodobenzonitrile (10.0 g, 43.7 mmol), sodium pentafluoroproprionate (15.4 g, 82.9 mmol), and copper(I) iodide (16.6 g, 87.3 mmol), DMF (160 mL), and toluene (60 mL) was heated at 160° C. for 16 h, allowing most of the toluene to distil off. After cooling, ethyl acetate (200 mL) was added, and the mixture was filtered through diatomaceous earth, and the filtrate was partitioned between ethyl acetate/heptane and water. The organic layer was washed with brine, dried (MgSO4), and evaporated. Chromatography (SiO2, heptane-ethyl acetate gradient) afforded the title compound (5.05 g 52%). Yellow oil, MS (EI) 221.1 (M+).

1. customto distil off
2. temperatureAfter cooling
3. additionethyl acetate (200 mL) was added
4. filtrationthe mixture was filtered through diatomaceous earth
5. customthe filtrate was partitioned between ethyl acetate/heptane and water
6. washThe organic layer was washed with brine
7. dry with materialdried (MgSO4)
8. customevaporated