摘要
以溴代二硝基甲烷钾盐和丙烯酸甲酯为原料,在相转移催化剂的作用下,通过Michael加成反应合成得到4-溴-4,4-二硝基丁酸甲酯。采用紫外光谱、红外光谱、核磁共振光谱、质谱以及元素分析等检测方法对目标化合物结构进行了表征。探讨了4-溴-4,4-二硝基丁酸甲酯的反应机理,并考察了反应温度、反应时间以及催化剂用量等对产物产率的影响规律。确定适宜的工艺条件为:反应物丙烯酸甲酯与溴代二硝基甲烷盐的投料摩尔比为2∶1,四丁基溴化铵的用量为溴代二硝基甲烷钾盐质量的12%,反应温度为40℃,反应时间为30 min,产物收率可达到54%。
Methyl-4-bromo-4,4-dinitrobutanoate was synthesized by Michael addition reaction of bromodinitromethane and methacrylate,and the effects of the ratio of raw materials,temperature and reaction time on its yield were studied. The optimum synthetic technology conditions with 54% yield are. molar ratio 2 ： 1 of methacrylate to bromodinitromethane potassium salt, reaction temperature 40 ℃, reaction time 30 min ,tetrabutyl ammonium bromide（TBAB） as phase transfer catalyst. The quantity of TBAB is equivalent to 12% of bromodinitromethane potassium salt. The structure of the product methyl-4-bromo-4,4-dinitrobu- tanoate was identified by infrared spectroscopy（IR）, nuclear magnetic resonance（^1 H NMR）, ultraviolet and visible spectroscopy （ UV-Vis）, mass spectroscopy（MS） and elemental analysis.
出处
《含能材料》
EI
CAS
CSCD
北大核心
2012年第1期22-25,共4页
Chinese Journal of Energetic Materials
基金
国家"973"资助项目(613830101-2)
国家自然科学基金资助项目(11076002)
