3-甲氧基丙烯酸甲酯的合成工艺研究.pdf

第47卷第2期
精细化工中间体
2017年4月
FINE CHEMICAL INTERMEDIATES
April 2017
农药及中
3-甲氧基丙烯酸甲酯的合成工艺研究
张革放12,胡志彬2,李谦和1,陈明2,王宇2,虞孝云“,柳爱平12
(1.湖南师范大学化学化工学院,湖南长沙410002.湖南化工研究院有限公司国家农药创例工程技
术研究中心,湖南沙410014;3.农用化学品湖南省重点实验室,湖南长沙410014;4.湖南海利
常徳农药化工有限公司,湖南常徳4150000
摘要:以四氟化碳和乙烯基乙为原料,在引发剂作用下发生自由基加成反应制备1,1
氧基两烷(以下简称丙烷化合物),丙烷化合物与甲醇回流得到3,3-二甲氧基两酸甲酯,然后在裂解催化
剂的作用下裂解为3-甲氧基两烯酸甲酯。优化エむ条件为:催化剂为偶気二异丁/间氯过氧萃甲酸,
(乙浠基乙醚):n(四氯化碳):n(偶氮二异丁睛):n(间氯过氧苯甲酸)=1:1.6:0.0016:0.0016,反应温度
为68℃,反应时间为6h;裂解反应所用催化剂为对甲苯磺酸。3步反应总收率为67、7%(以を烯基乙誌
计),含量为98.5%。
关键词:四氯化碳;自由基加成;3,3-二甲氧基丙酸甲指
中图分类号:TY225.24文献标志码:A文章编号:1009-9212(2017)02-0025-04
DOI:10.19342/ i cnki. issn.1009-9212.2017.02.005
Synthesis of Methyl 3-methoxyacrylate
ZHANG Gefang HU.! ian-he CHENG Ming, WA N Yuyuxi-unluai-ing
(1. College of Chemistry and Chemical Engineering, Hunan Normal University, Changsha 410006, China; 2. National
Engineering Research Center for Agrochemicals, Hunan Research Institute of Chemieal Industry Co, Ltd, Changsha
410014. China; 3. Ilunan Province Key Laboratory for Agrochemicals, Changsha 410014, China; 4. Hunan Haii
Changde Pesticide Chemical Industry Co, Ltd, Changde 415000, China)
Abstract: Methyl 3-methox acrylate was pyrolyzed by methyl 3, 3-dimethoxy-propionate, which was successful
synthesized from the reflux of I, 1, 1, 3-1etrachloro-3-ethoxy-propane in methanol. 1, 1, 1. 3-tetrachloro-3-ethoxy
propane was prepared using vinyl ether and carbon tetrachloride as the raw materials, AIBN and 3
chloroperbenzoic acid as catalysts. The optimum conditions for synthesis of 1, 1, 1,3-tetrachloro-3-elhoxypropanc
were as followings: n(vinyl ether]: n(carbon tetrachloride: n(AIBN): (3-chloroperbenzoic acid) was of 1: 1.6: 0.0016
0.0016; reaction temperature was of 68; reaction timc was of 6 h; the eracking catalyst was p-toluenesulfonic
acid. The overall yield of the target compound reached 67.7%o with a purity of 98.5%o
Key words carbon tetrachloride free radical addition; intermediates; Synthesis methyl 3, 3-dimethoxypropionate
前言
成中重要的C-3砌块,应用于农药、医药、高分
子材料等领域。用于合成多种有机化合物,如头孢
3-甲氧基丙烯酸甲酯为无色透明液体,是多
布烯、氟啶虫酰胺?、马钱苷.3、杀菌剂硅菌
官能闭化合物,具有很好的反应活性,是有机合胺列、1-氨基-2-毗略-3-磯胶酯以及除草剂1
基金项目:家月然科学基金(21572050)
作者简介:张革放(1993-),男,湖南荒阳人,硕土钘究生,研究方向:有机合成
联系人:胡志彬、博土,研究方向:有机合或(E-mail:gushantox(163.com)
收稿日期:2017-04-10
万方数据