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微波辐射法合成单琥珀酸薄荷酯

Synthesis of Monomenthyl Succinate Under Microwave Radiation

  • 摘要: 为寻求单琥珀酸薄荷酯的更优合成方法,在微波辐射下,以HClO4-SiO2作催化剂,丁二酸酐和薄荷醇为原料合成了单琥珀酸薄荷酯,利用IR,1H NMR,13C NMR对其结构进行了表征;采用正交试验设计优化了合成条件,并与传统合成方法进行了对比。结果表明:①合成产物为目标物;②合成单琥珀酸薄荷酯的最优条件为:微波功率400 W,反应时间14 min,丁二酸酐、薄荷醇与催化剂的摩尔比1.2:1:0.012,在此条件下单琥珀酸薄荷酯的产率平均为90.1﹪;③HClO4-SiO2催化剂可以重复使用3~4次。微波辐射下,以HClO4-SiO2为催化剂是一种合成单琥珀酸薄荷酯的高效简便的方法。

     

    Abstract: In order to find a better method for synthesizing monomenthyl succinate,the compound was synthesized by subjecting the starting materials,succinic anhydride and menthol to microwave radiation in the presence of HClO4-SiO2 as a catalyst. The structure of the resultant compound was characterized by IR,1H NMR and 13C NMR. The synthesis parameters were optimized by orthogonal test and compared with traditional synthesis method. The results showed that:1) The synthesized compound was the target product. 2) The optimum condition was microwave power 400 W,reaction time 14 minutes,mole ratio of succinic anhydride to menthol to HClO4-SiO2 1.2:1:0.012,under which the average yield of the compound was 90.1%. 3)HClO4-SiO2 could be reused for 3 to 4 times. Under microwave radiation and taking HClO4-SiO2 as a catalyst was an efficient and simple way for the synthesis of monomenthyl succinate.

     

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