树枝化聚合物原料——3,5-二溴苯甲酸乙酯的合成研究  

Study on Synthesis of Ethyl 3,5-Dibromobenzoate as Raw Material for Preparing Dendritic Polymers

作　　者：陈林[1] 徐立[1] 邵立东[1] 胡敏奇[1] 何锋[1] 毕韵梅[1] 

机构地区：[1]云南师范大学化学化工学院,云南昆明650500

出　　处：《化学世界》2011年第3期166-168,共3页Chemical World

基　　金：国家自然科学基金(20864003);云南省社会发展科技计划应用基础研究专项面上项目(2009ZC064M)

摘　　要：在乙酸乙酯介质中,3,5-二溴-4-氨基苯甲酸乙酯经重氮化和还原脱氨一步法合成树枝化聚合物原料—3,5-二溴苯甲酸乙酯,通过正交实验得到3,5-二溴苯甲酸乙酯的最佳合成条件为:硫酸用量为3,5-二溴-4-氨基苯甲酸乙酯的2.5倍,反应温度为60℃,3,5-二溴-4-氨基苯甲酸乙酯与亚硝酸钠的摩尔比为1∶3,乙酸乙酯用量为反应物总体积的8倍,产率94%。该方法减少了合成步骤,缩短了反应时间,产物分离纯化简便,产率高。Ethyl 3,5-dibromobenzoate as raw material used to prepare dendritic polymers was synthesized from ethyl 4-amino-3,5-dibromobenzoate through diazotization and reductive deamination by one-step in ethyl acetate medium.The optimum conditions of synthesizing the title compound by orthogonal test were obtained as follows： the molar ratio of sulfuric acid to ethyl 4-amino-3,5-dibromobenzoate was 2.5∶1;the reaction temperature was 60℃;the molar ratio of 4-amino3,5-dibromobenzoate to sodium nitrite was 1∶3;ethyl acetate was added in an amount of eight times the volume of all reagents.Under the optimum synthetic conditions,the yield of the product was 94%.The method reduced reaction steps,shortened reaction time and raised the yield.The product could be purified easily.

关 键 词：3 5-二溴苯甲酸乙酯 脱氨基 正交实验 合成 

分 类 号：O625[理学—有机化学]