| 4,4-二硝基丁酸乙酯的合成研究 |
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| 引用本文： | 黄婷,金波,彭汝芳,肖玲娜,楚士晋.4,4-二硝基丁酸乙酯的合成研究[J].西南科技大学学报,2014(4):5-8. |
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| 作者姓名： | 黄婷 金波 彭汝芳 肖玲娜 楚士晋 |
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| 作者单位： | 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 |
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| 基金项目： | 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） |
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| 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%。
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| 关 键 词： | 相转移催化剂 Michael加成反应 4 4-二硝基丁酸乙酯 |
On Synthesis of Ethyl 4, 4 - dinitrobutanoate |
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| Institution: | HUANG Ting, JIN Bo, PENG Ru - fang, XIAO Ling - na, CHU Shi - jin (State Key Laboratory Cultivation Base for Nonmetal Composites and Functional Materials, Southwest University of Science and Technology, Mianyang 621010, Sichuan , China) |
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| Abstract: | 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. |
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| Keywords: | Phase transfer catalyst Michael addition reaction Ethyl 4 4 -dinitrobutanoate |
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