摘要
以溴代二硝基甲烷钾盐和丙烯酸乙酯为原料,在相转移催化剂四丁基溴化铵的作用下通过Michael加成反应得到4-溴-4,4-二硝基丁酸乙酯。通过单因素实验,探讨了反应物料摩尔比、反应温度、反应时间及催化剂用量对产物产率的影响,得到的最佳工艺条件为:反应温度30℃,n(丙烯酸乙酯)∶n(溴代二硝基甲烷钾盐)=2∶1,反应时间30 min,四丁基溴化铵用量为溴代二硝基甲烷钾盐物质的量的20%,在该条件下产物产率可达52%;并用UV-vis、FTIR、1HNMR、MS以及元素分析等方法表征了产物的结构。
Ethyl 4-bromo-4, 4-dinitrobutyrate was synthesized by Michael addition reaction of bromodinitromethane potassium salt with ethyl acrylate, and the effect of the ratio of raw materials, reaction temperature and time on the yield of the target product was studied through a single factor experiment. The optimum synthesis conditions with a yield of 52% are：molar ratio 2：1 of ethyl acrylate to bromodinitromethane potassium salt, reaction temperature 30 ℃ ,reaction time 30 min, and TBAB as phase transfer catalyst. The quantity of TBAB is equivalent to 20% of bromodinitromethane potassium salt. The structure of the product ethyl 4-bromo-4,4-dinitrobutanoate was identified by means of IR, ^1HNMR, UV-vis, MS and elemental analysis.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2011年第11期1141-1144,共4页
Fine Chemicals
基金
国家"973"资助项目(613830101-2)
国家自然科学基金资助项目(11076002)~~
