反应 #3541877
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US05210315
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: In a 50 ml flask equipped with a thermometer, a dropping funnel, and a stirrer were charged 7 ml of methylene chloride, 7 ml of water, 2 mmole of 1-methyl-1-cyclohexene, and 0.1 mmole of each of ruthenium catalysts shown in Table 2 below. To the mixture was added dropwise a 30% ethyl acetate solution of 1.52 g (6 mmole) of peracetic acid at room temperature over 2 hours while stirring on a magnetic stirrer. After the addition, the stirring was further continued at room temperature for 2 hours. The reaction mixture was extracted three times with 20 ml portions of methylene chloride. The extract was washed with 30 ml of a saturated sodium chloride aqueous solution and dried over anhydrous magnesium sulfate. The solvent was removed by distillation, and the residual crude product was purified by silica gel column chromatography using a 5:1 (by volume) mixture of n-hexane and ethyl acetate as an eluent to obtain 2-methyl-2-hydroxy-1-cyclohexanone. The percent yield of the product is shown in Table 2. In a 50 ml flask equipped with a thermometer, a dropping funnel, and a stirrer After the addition The reaction mixture was extracted three times with 20 ml portions of methylene chloride The extract was washed with 30 ml of a saturated sodium chloride aqueous solution dried over anhydrous magnesium sulfate The solvent was removed by distillation the residual crude product was purified by silica gel column chromatography a 5:1 (by volume) mixture of n-hexane and ethyl acetate as an eluent
来源 ID: ord-776dcd429e524bf6ba2341d516752278