反应 #3023457
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US09035059B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A solution of 2-(4-tert-butylphenyl)ethanol (5.35 g, 30.0 mmol) in chloroform (150 mL) was cooled in ice and Dess-Martin periodinane (16.5 g, 39.0 mmol) was added thereto. The mixture was warmed to room temperature and stirred for 3 hr. The reaction mixture was diluted with chloroform (150 mL), followed by cooling in ice. Thereafter, saturated aqueous sodium thiosulfate solution was added thereto and the mixture was stirred for 5 min. The mixture was extracted three times with chloroform and then the organic layer was washed with brine and dried over anhydrous magnesium sulfate. The desiccant was filtered off and then the filtrate was concentrated under reduced pressure. The resulting precipitate was filtered again, followed by washing with chloroform. The filtrate was concentrated under reduced pressure and the resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=9:1) to afford the title compound as a yellow oil (4.24 g). by cooling in ice the mixture was stirred for 5 min The mixture was extracted three times with chloroform the organic layer was washed with brine dried over anhydrous magnesium sulfate The desiccant was filtered off the filtrate was concentrated under reduced pressure The resulting precipitate was filtered again by washing with chloroform The filtrate was concentrated under reduced pressure the resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=9:1)
来源 ID: ord-2074c7fe8f0340458aeb70fe936da491