反应详情

温度

55 °C

In ethanol (4 ml) were dissolved (3S)-2-(2,4-difluorophenyl)-3-(3,4,5,6-tetrahydro-2H-pyran-2-yl)oxy-1-(1H-1,2,4-triazol-1-yl)-2-butanol (0.22 g) and pyridinium p-toluenesulfonate (47 mg), which was stirred for two hours at 55° C. To the solution was further added pyridinium p-toluenesulfonate (10 mg), which was stirred for further two hours at 55° C. The reaction mixture was cooled, then the solvent was distilled off. To the residue was added ethyl acetate (30 ml), which was washed with a saturated aqueous sodium chloride solution (10 ml). The ethyl acetate layer was dried over anhydrous magnesium sulfate, then the solvent was distilled off under reduced pressure. To the residue was added ethyl ether, then precipitating crystals were collected by filtration to obtain (2S,3S)-2-(2,4-difluorophenyl)-1-(1H-1,2,4-triazol-1-yl)-2,3-butanediol (60 mg). m.p. 115°-117° C.

1. stirringwas stirred for further two hours at 55° C
2. temperatureThe reaction mixture was cooled
3. distillationthe solvent was distilled off
4. additionTo the residue was added ethyl acetate (30 ml), which
5. washwas washed with a saturated aqueous sodium chloride solution (10 ml)
6. dry with materialThe ethyl acetate layer was dried over anhydrous magnesium sulfate
7. distillationthe solvent was distilled off under reduced pressure
8. additionTo the residue was added ethyl ether
9. customprecipitating crystals
10. filtrationwere collected by filtration