微波辐射法合成单琥珀酸薄荷酯

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。

Synthesis of Monomenthyl Succinate Under Microwave Radiation

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.