反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
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.
WORKUP
后处理
- customIn a 50 ml flask equipped with a thermometer, a dropping funnel, and a stirrer
- additionAfter the addition
- extractionThe reaction mixture was extracted three times with 20 ml portions of methylene chloride
- washThe extract was washed with 30 ml of a saturated sodium chloride aqueous solution
- dry with materialdried over anhydrous magnesium sulfate
- customThe solvent was removed by distillation
- customthe residual crude product was purified by silica gel column chromatography
- additiona 5:1 (by volume) mixture of n-hexane and ethyl acetate as an eluent