4,4–二硝基丁酸甲酯的合成工艺研究  

Synthesis Technology of Methyl 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]四川省非金属复合与功能材料重点实验室,西南科技大学,四川绵阳621010

出　　处：《化学推进剂与高分子材料》2013年第5期59-62,81,共5页Chemical Propellants & Polymeric Materials

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：以二硝基甲烷钾盐与丙烯酸酯为反应原料,四丁基溴化铵为相转移催化剂,通过Michael加成反应合成得到4,4–二硝基丁酸甲酯。采用核磁共振氢谱、红外光谱、紫外–可见光谱、质谱及元素分析等对产物结构进行了表征。通过单因素方法,探讨了反应时间、反应温度、催化剂用量及反应物料比对产物产率的影响,得到该反应的最佳工艺条件:以四丁基溴化铵为相转移催化剂,反应温度为35℃,n(丙烯酸甲酯)︰n(二硝基甲烷钾盐)为3︰1,反应时间为30 min,四丁基溴化铵的质量为二硝基甲烷钾盐的10%,产物偕二硝基丁酸甲酯收率可达29%。The methyl 4,4-dinitrobutanoate was obtained through Michael addition reaction using potassium salt of dinitromethane and methyl acrylate as reaction materials and tetrabutyl ammonium bromide as phase transfer catalyst. The structure of product was characterized by using IH-NMR, IR, UV-vis, mass spectrum, element analysis, and so on. The influence of reaction time, reaction temperature, catalyst amount and reactant ratio on yield of product was discussed through single factor method. The obtained optimal process conditions are as follows： using tetrabutyl ammonium bromide as phase transfer catalyst, reaction temperature is 35 ℃, n（methyl acrylate） ： n（potassium salt of dinitromethane）=3 ：l, reaction time is 30 min, the mass of tetrabutyl ammonium bromide is 10% of potassium salt of dinitromethane mass. The yield of methyl gem-dinitrobutanoate product can reach 29% under the above optimal reaction conditions.

关 键 词：4 4-二硝基丁酸甲酯 相转移催化剂 MICHAEL加成反应 

分 类 号：TQ414[化学工程]