3,4-亚甲二氧基苯甲酸乙酯的合成与正交试验

Synthesis and Orthogonal Test of 3,4-Methylenedioxy Benzoic Acid Ethyl Ester

3,4-亚甲二氧基苯甲酸(胡椒酸)和乙醇为原料,以浓硫酸为催化剂合成了3,4-亚甲二氧基苯甲酸乙酯(胡椒酸乙酯),其结构经~1H NMR,^(13)C NMR和IR表征。采用单因素和正交试验对其合成条件进行了优化,得到最佳合成条件:浓硫酸用量为25%[m(催化剂)∶m(胡椒酸)=0.25],回流反应时间20h,反应温度85℃,3,4-亚甲二氧基苯甲酸乙酯产率达到89%。

3,4-Methylenedioxybenzoic acid ethyl ester（piperic acid ethyl ester）was prepared from 3,4-Methylenedioxybenzoic acid（piperic acid）and ethanol using H2SO4 as catalyst and characterized by 1H NMR,13C NMR,and IR.Single factor and orthogonal tests were employed to optimize the synthetic technology.The optimal reaction conditions are as follows：concentrated sulfuric acid as catalyst,the amount of catalyst：25%,reaction time 20 h,and reaction temperature：85 ℃.Under the optimum conditions,the yield of 3,4-methylenedioxybenzoic acid ethyl ester could reach as high as 89%.