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以环己酮为底物、30%H2O2为氧源、钨酸钠为催化剂,首次采用无机盐硫酸氢钠为酸性配体催化合成了标题化合物。结果表明,该反应体系具有成本低、无有害物排放、不易腐蚀设备、催化剂和酸性配体易分离回收并可重复使用等优点。考察了催化剂用量、配体用量、H2O2用量及反应时间等因素对产物收率的影响,确定了适宜反应条件为n(环己酮)∶n(H2O2)∶n(钨酸钠)∶n(硫酸氢钠)=1∶4.94∶0.02∶0.02,反应时间6 h,收率达82.2%。实验还发现,采用硫酸氢钾、氨基磺酸及对甲苯磺酸为酸性配体适宜反应条件下收率分别为83.6%、81.5%和71.2%,同样显示出上述优越性。
The title compound was synthesized using cyclohexanone as the substrate, 30% H2O2 as the oxygen source and sodium tungstate as the catalyst for the first time using inorganic sodium bisulfate as acidic ligand. The results show that the reaction system has the advantages of low cost, non-hazardous emissions, non-corrosive equipment, easy separation and recovery of catalyst and acidic ligands. The effects of the amount of catalyst, the amount of ligand, the amount of H2O2 and the reaction time on the yield of the product were investigated. The optimum reaction conditions were as follows: n (cyclohexanone): n (H2O2): n Sodium bisulfate) = 1: 4.9: 0.02: 0.02, the reaction time was 6 h and the yield was 82.2%. The experiment also found that the use of potassium bisulfate, sulfamic acid and p-toluenesulfonic acid as the acidic ligand yield under appropriate conditions were 83.6%, 81.5% and 71.2%, also shows the above advantages.