反应详情

温度

15 °C

To dimethyl sulfoxide (5 ml) was added 60% sodium hydride in oil (85 mg), to which was added trimethyl sulfoxonium iodide (0.49 g) with stirring at about 15° C., and the mixture was stirred for 15 minutes at room temperature. The reaction mixture was cooled with ice, to which was added a dimethyl sulfoxide solution (1.2 ml) of (2S)-2',4'-difluoro-2-(3,4,5,6-tetrahydro- 2H-pyran-2-yloxy)propiophenone (0.50 g), and the mixture was stirred for two hours at room temperature. To the reaction mixture were added water (10 ml) and ethyl acetate (50 ml), and the resultant mixture was shaken. The organic layer was washed with a saturated aqueous sodium chloride solution (10 ml) twice, which was dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, and the residue was purified by means of a silica gel chromatography (eluent, hexane:ethyl acetate=10:1) to afford 2-[(1S)-1-(3,4,5,6-tetrahydro-2H-pyran-2-yloxy)ethyl]-2-(2,4-difluorophenyl)oxirane (0.40 g) as a pale yellow oily product.

1. stirringthe mixture was stirred for 15 minutes at room temperature
2. temperatureThe reaction mixture was cooled with ice, to which
3. stirringthe mixture was stirred for two hours at room temperature
4. washThe organic layer was washed with a saturated aqueous sodium chloride solution (10 ml) twice
5. dry with materialwhich was dried over anhydrous magnesium sulfate
6. distillationThe solvent was distilled off under reduced pressure
7. customthe residue was purified by means of a silica gel chromatography (eluent, hexane:ethyl acetate=10:1)