4,4-二硝基丁酸乙酯的合成研究  

On Synthesis of Ethyl 4,4- dinitrobutanoate

作　　者：黄婷[1] 金波[1] 彭汝芳[1] 肖玲娜[1] 楚士晋[1] 

机构地区：[1]西南科技大学四川省非金属复合与功能材料重点实验室-省部共建国家重点实验室培育基地,四川绵阳621010

出　　处：《西南科技大学学报》2014年第4期5-8,共4页Journal of Southwest University of Science and Technology

基　　金：国家自然科学基金委员会-中国工程物理研究院NSAF联合基金重点资助项目(10576026);国防基础科研项目(A3120110005;A3120133002)

摘　　要：以丙烯酸乙酯与二硝基甲烷钾盐为反应原料,四丁基溴化铵为相转移催化剂,通过Michael加成反应合成4,4-二硝基丁酸乙酯。采用红外光谱、紫外可见光谱、质谱、核磁共振氢谱及元素分析等对产物结构进行了表征。通过单因素变量法探讨了反应时间、反应物料比、催化剂用量及反应温度对产物产率的影响,得出该反应最佳工艺条件:反应时间为60 min,反应温度为20℃,n丙烯酸乙酯:n二硝基甲烷钾盐为2:1,相转移催化剂四丁基溴化铵质量为二硝基甲烷钾盐质量的30%时,产物偕二硝基丁酸乙酯收率可达到33%。Ethyl 4,4 -dinitrobutanoate was successfully synthesized by Michael addition reaction of dini- tromethane potassium salt and ethacrylate. The structure of the product Ethyl 4, 4 - dinitrobutanoate was identified by IR, UV - Vis, MS, 1H NMR and elemental analysis. And the effects of the reaction time, the ratio of raw materials and time on the reaction were studied. The optimum synthetic technology conditions with 33% yield of ethyl 4, 4 -dinitrobutanoate are： the reaction time is 60 min, the reaction temperature is 20 ℃, the molar ratio of methacrylate to dinitromethane potassium salt is 2 ： 1, with TBAB as the phase transfer catalyst. The quality of TATB is equivalent to 30% of dinitromethane potassium salt.

关 键 词：相转移催化剂 MICHAEL加成反应 4 4-二硝基丁酸乙酯 

分 类 号：O621.3[理学—有机化学]