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.
出处
《合成化学》
CAS
CSCD
北大核心
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)
