负载型KMnO_4的制备及其在低蒎酮酸合成中的应用  

Preparation of Supported KMnO_4 and Their Application in the Synthesis of Pinononic Acid

作　　者：孙小玲[1] 王蕊[1,2] 

机构地区：[1]上海应用技术学院化学与环境工程学院,上海200235 [2]上海海洋大学食品学院,上海201306

出　　处：《合成化学》2011年第3期389-392,共4页Chinese Journal of Synthetic Chemistry

基　　金：上海市重点学科建设基金资助项目(J1503);上海市高校特聘教授(东方学者)岗位计划资助项目(DF2009-02);上海市教委研究生创新能力培养专项资金资助项目(YC200905);上海应用技术学院科技发展基金资助项目(KJ2008-08)

摘　　要：分别以硅酸铝、分子筛、石墨、硅藻土、硅胶、中性氧化铝、二氧化锰为载体,制备了七种负载型KMnO4(1a～1g),其结构经XRD表征。以1为氧化剂,马鞭草烯酮的碳碳双键完成氧化断裂反应,合成了一种重要的杀虫剂中间体低蒎酮酸(2),其结构经1H NMR和IR确证。合成2的较适宜反应条件为:马鞭草烯酮13.3mmol,1e10.32 g(40 mmol,以KMnO4计算),91%AcOH 50 mL,于室温反应2 h,转化率100%,选择性81.04%。Seven kinds of supported KMnO4（1a～1g） were prepared using aluminium silicate,molecular sieve,graphite,kieselguhr,silica-gel,alumina and manganese dioxide as support,respectively.The structures were characterized by XRD.An important pesticide intermediate,pinononic acid（2）,was synthesized by the carbon-carbon double bond cleavage of verbenone using 1 as oxidant.The structure of 2 was confirmed by 1H NMR and IR.The appropriate reaction conditions at room temperature for 2 h for synthesizing 2 were as follows： verbenone 13.3 mmol,1e 10.32 g（40 mmol,calcd for KMnO4）,91%AcOH 50 mL.The conversion and selectivity reached 100% and 81.04% under the conditions,respectively.

关 键 词：负载型KMnO4 氧化剂 马鞭草烯酮 低蒎酮酸 合成 

分 类 号：O621.25[理学—有机化学]