反应详情

10% hydrogen peroxide (10.5 ml, 0.023 mol) was added dropwise to a stirred, refluxing solution of 2,3 -difluoro-4 -octoxybiphenyl-4'-yl-boronic acid (10) (2.9g, 8.0 mmol), in diethyl ether (40 ml). The stirred mixture was heated under reflux until tic showed the reaction to be complete. The ether layer was separated and the aqueous layer extracted with ether. The combined ethereal layers were washed with water and dried. The solvent was removed. The crude product was purified by flash chromatography (silica gel/petroleum fraction (bp 40°-60° C.) - ethyl acetate, 2:1) to give a white solid which was recrystallised from pentane/ethyl acetate mixtures.

1. temperatureThe stirred mixture was heated
2. temperatureunder reflux
3. customthe reaction
4. customThe ether layer was separated
5. extractionthe aqueous layer extracted with ether
6. washThe combined ethereal layers were washed with water
7. customdried
8. customThe solvent was removed
9. customThe crude product was purified by flash chromatography (silica gel/petroleum fraction (bp 40°-60° C.) - ethyl acetate, 2:1)
10. customto give a white solid which
11. customwas recrystallised from pentane/ethyl acetate mixtures