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| 相转移催化法合成4-溴-4,4-二硝基丁酸甲酯 | |
| 引用本文： | 肖玲娜,金波,彭汝芳,史文秀,楚士晋,董海山.相转移催化法合成4-溴-4,4-二硝基丁酸甲酯[J].含能材料,2012,20(1):22-25. |
| 作者姓名： | 肖玲娜 金波 彭汝芳 史文秀 楚士晋 董海山 |
| 作者单位： | 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 2. 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;北京理工大学化工与环境学院,北京100081 3. 北京理工大学化工与环境学院,北京100081;中国工程物理研究院化工材料研究所,四川绵阳621900 |
| 基金项目： | 国家“973”资助项目(613830101-2); 国家自然科学基金资助项目(11076002) |
| 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%。 |
| 关 键 词： | 有机化学 4-溴-4 4-二硝基丁酸甲酯 Michael加成反应 相转移催化剂 |
| 收稿时间： | 1/4/2011 12:00:00 AM |
| 修稿时间： | 7/20/2011 4:56:53 PM |
Synthesis of Methyl-4-bromo-4, 4-dinitrobutyrate by Phase Transfer Catalysis |
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| XIAO Ling-n,JIN Bo,PENG Ru-fang,SHI Wen-xiu,CHU Shi-jin and DONG Hai-shan.Synthesis of Methyl-4-bromo-4, 4-dinitrobutyrate by Phase Transfer Catalysis[J].Chinese Journal of Energetic Materials,2012,20(1):22-25. | |
| Authors: | XIAO Ling-n JIN Bo PENG Ru-fang SHI Wen-xiu CHU Shi-jin and DONG Hai-shan |
| Affiliation: | State Key Laboratory Cultivation Base for Nonmetal Composites and Functional Materials, Southwest University of Science and Technology, Mianyang 621010, China;;State Key Laboratory Cultivation Base for Nonmetal Composites and Functional Materials, Southwest University of Science and Technology, Mianyang 621010, China; 2. School of Chemical Engineering and Environment, Beijing Institute of Technology, Beijing 100081, China;;State Key Laboratory Cultivation Base for Nonmetal Composites and Functional Materials, Southwest University of Science and Technology, Mianyang 621010, China;;State Key Laboratory Cultivation Base for Nonmetal Composites and Functional Materials, Southwest University of Science and Technology, Mianyang 621010, China;;State Key Laboratory Cultivation Base for Nonmetal Composites and Functional Materials, Southwest University of Science and Technology, Mianyang 621010, China;;School of Chemical Engineering and Environment, Beijing Institute of Technology, Beijing 100081, China; 3. Institute of Chemical Materials, China Academy of Engineering Physics, Mianyang 621900, China |
| Abstract: | 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-dinitrobutanoate was identified by infrared spectroscopy(IR),nuclear magnetic resonance(1H NMR),ultraviolet and visible spectroscopy(UV-Vis),mass spectroscopy(MS) and elemental analysis. |
| Keywords: | organic chemistry methyl-4-bromo-4 4-dinitrobutanoate Michael addition reaction phase transfer catalyst |
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