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4-三氟甲基烟酸的合成工艺设计

时间:2019-03-30 14:51来源:毕业论文
设计了4-三氟甲基烟酸的合成路线:以三氟乙酰乙酸乙酯和氰基乙酰胺为原料,通过环合、氯化、氰基水解、催化氢解四步反应得到4-三氟甲基烟酸。改进以后的方法产率高,反应条件温

摘要4-三氟甲基烟酸是含三氟甲基的含氮杂环化合物,他们在生物体内具有独特的生理活性而受到广泛关注,可以作为制备其他很多药物的前体物质。它们具有独特的作用机理,极高的生物活性,能更有效的杀死害虫并且对温血动物的毒性很小,同时也能克服虫类对其他农药抗药性的难题,因此研究4-三氟甲基烟酸的合成工艺具有重大的现实意义。33994
本文通过查阅文献,结合成本,工业化生产的难易程度,设计了4-三氟甲基烟酸的合成路线:以三氟乙酰乙酸乙酯和氰基乙酰胺为原料,通过环合、氯化、氰基水解、催化氢解四步反应得到4-三氟甲基烟酸。改进以后的方法产率高,反应条件温和,每步产物容易分离提纯,适合工业化生产。
通过实验来探索合成的最佳条件,优化工艺,并确定合成路线的可行性。实验过程中的每步产物通过红外、质谱、核磁等手段进行表征。
关键词  4-三氟甲基烟酸;三氟乙酰乙酸乙酯;氰基乙酰胺合成
毕业论文设计说明书外文摘要
Title  Study on the Synthetical Technology of 4-(Trifluoromethyl)nicotinic Acid                                                 
Abstract
4-trifluoromethylnicotinic acid is useful as the precursors for production of agricultural chemicals or pharmaceuticals due to their biologically activity. Some compounds derived from 4-trifluoromethylnicotinic can be used as active ingredients for pesticides directly. They are able to protect fish, shellfish and domestic animals from the harmfulness because unique mechanism and high biologically activity. In addition, they are also overcome the hard problem of the resistance of pests to other pesticide. Therefore, it is of great practical value to research on synthesis of 4-trifluoromethylnicotinic acid. 源`自*六)维[论*文'网www.lwfree.cn
A possible synthesis method is designed in this dissertation according to the reference. Starting from trifluoroacetoacetate and cyanoacetamide, via cyclization, chlorination, hydrolysis, hydrogenolysis, 4-trifluoromethylnicotinic acid was obtained. This method has the following advantages : satisfactory yield ,easy purification, low equipment requirements and suitability for industrial production.
Each step was optimized during Synthesis processes. The most effective conditions were determined  through single factor experiments. Each intermediate was characterized by the melting point determination, MS, NMR. The results proved the structures of the products conformed to the target products.
Keywords  4-trifluoromethylnicotinic acid; trifluoroacetoacetate; cyanoacetamide; Synthesis
目   次
1  绪论    1
1.1  概述    1
1.1.1  烟酸的结构、性质及用途    1
1.1.2  含氟化合物的生物活性    2
1.1.3  含氟化合物的应用    3
1.1.4  近年来烟酸与含氟化合物的发展    5
1.2 合成方法    6
1.2.1  引入含氟基团的方法    6
1.2.2  4-三氟甲基烟酸的合成方法    7
1.3  本文研究内容    8
2  实验部分    10
2.1  一般实验条件    10
2.1.1  一般仪器    10
2.1.2  分析仪器    10
2.1.3  色谱分离    10
2.1.4  实验试剂    11
2.2  实验方法    11
2.2.1  2,6-二羟基-4-三氟甲基烟腈的制备    11 4-三氟甲基烟酸的合成工艺设计:http://www.lwfree.cn/huaxue/20190330/31344.html
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