反应详情

温度

55 °C

In ethanol (3 ml) was dissolved (2R)-2',4'-difluoro-2-(3,4,5,6-tetrahydro-2H-pyran-2-yloxy)propiophenone (121 mg), to which was added pyridinium p-toluenesulfonate (25 mg), and the mixture was stirred for one hour at 55° C. The solvent was distilled off under reduced pressure, and the residue was dissolved in ethyl acetate (20 ml). The solution was washed with water and dried over anhydrous magnesium sulfate, followed by distilling off the solvent. The residue was purified by means of a silica gel chromatography (eluent: hexane-ethyl acetate=5:1) to give (2R)-2',4'-difluoro-2-hydroxypropiophenone (62 mg) as a pale yellow oily product. [α]D +68.7 (c=1.8 in chloroform)

1. distillationThe solvent was distilled off under reduced pressure
2. dissolutionthe residue was dissolved in ethyl acetate (20 ml)
3. washThe solution was washed with water
4. dry with materialdried over anhydrous magnesium sulfate
5. distillationby distilling off the solvent
6. customThe residue was purified by means of a silica gel chromatography (eluent: hexane-ethyl acetate=5:1)