反应详情

温度

130 °C

Add potassium carbonate (27.4 g, 198 mmol) to a mixture of 4-fluorobenzonitrile (8 g, 66 mmol) and (±)-3,3,4,4,4-pentafluoro-2-butanol (17.2 g, 105 mmol) in anhydrous DMF (60 mL). Heat the mixture in a sealed flask for 4 h at 130° C. Cool the reaction to ambient temperature, dilute with hexane/EtOAc (1:1, 350 mL) and wash with aqueous 5% sodium chloride (3×100 mL). Collect the organic layer, dry over Na2SO4, filter and concentrate in vacuo to obtain the desired intermediate (17.1 g, 98%). GC-MS m/z: 432 (M+).

1. temperatureCool
2. customthe reaction to ambient temperature
3. washwash with aqueous 5% sodium chloride (3×100 mL)
4. customCollect the organic layer
5. dry with materialdry over Na2SO4
6. filtrationfilter
7. concentrationconcentrate in vacuo