反应详情

温度

170 °C

The 2,5-difluorophenol allyl ether (13 g) was dissolved in N,N-dimethylaniline (90 ml) and the resulting solution was stirred under a nitrogen gas stream at 170° C. for 5 hr. Then the liquid reaction mixture was poured into a 10% aqueous solution of hydrogen chloride and extracted with ethyl acetate. The organic layer was washed with brine, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (developing solvent: 7% ethyl acetate/n-hexane) to give 2-allyl-3,6-difluorophenol (7.8 g) as a colorless oil.

1. customThen the liquid reaction mixture
2. extractionextracted with ethyl acetate
3. washThe organic layer was washed with brine
4. dry with materialdried over anhydrous magnesium sulfate
5. concentrationconcentrated under reduced pressure
6. customThe resulting residue was purified by silica gel column chromatography (developing solvent: 7% ethyl acetate/n-hexane)