摘 要：脒类化合物在农药和医药中被广泛应用，本文主要针对现有的合成方法进行改进，并合成了N,N-二乙基间甲基苯甲脒、N,N-二乙基对氯苯甲脒和N,N-二乙基对甲基苯甲脒。
本文主要运用无催化、无溶剂的密闭加压体系合成了脒类化合物，且原料易得，反应简单，对环境友好。通过比较反应在不同温度下,不同投料比,以及不同原料的条件下,选出了最优工艺路线。并且对不同取代甲酰苯胺的反应活性有了初步结论：间甲基甲酰苯胺>对甲基甲酰苯胺>对氯甲酰苯胺。35484
反应的最优工艺路线为：在55℃下，将间甲基甲酰苯胺与二乙胺按摩尔比1:4投入反应，加入三氯氧磷作为脱水剂，反应5-6小时，得到产率为84%的N,N-二乙基间甲基苯甲脒。
毕业论文关键词：N,N-二乙基取代苯甲脒、二乙胺、无催化、无溶剂、合成
No catalytic melting synthesis of amidines
Abtract: Amidine compounds are widely used in pesticide and medicine, this article mainly aims at the existing synthesis method was improved, and the synthesis of N, N - diethyl methyl benzoic between amidine, N, N - diethyl chlorobenzene amidine and N, N - diethyl methyl benzene armour amidine.
In this paper, we use without catalyst and solvent confined compression system amidine compounds were synthesized, and the reactants, reaction is simple, friendly to environment. The optimal technological route was selected by the comparison of the reaction temperature and the ratio of feed to feed and the conditions of different raw materials. And the reaction activity of different substituted for the aniline was preliminarily concluded. The reaction activity about different substituted for the aniline is m-methylformanilide> p-methylformanilide > p-chloroformanilide.
The optimal process route for the reaction is that at 55℃ m-methyl formanilide and diethylamine molar of 1:4 into reaction, and adding phosphorus oxychloride as dehydrating agent, reactin of 5-6 hours, get N, N - diethyl methyl benzoic between amidine about the yield was 84%.
Keywords: N, N - diethyl substituted benzamidine, diethylamine, catalysis, solvents, synthesis
目 录
1.前言1
1.1脒类化合物的简介•••1
1.2脒类化合物的用途•••1
1.3 脒类化合物的前景•••2
1.4 脒类化合物的合成方法•••2
1.4.1酰胺法••3
1.4.2腈的氨解法••3
1.4.3改进的Pinner法•4
1.4.4氨基还原固相合成法••5
1.4.5 Sm/TMSCl/H2O微量体系6
1.4.6由酯合成脒••7
1.5 脒及其化合物的应用••7
1.5.1环脒的应用••8
1.5.2聚脒的应用••8
1.6 本课题的研究意义与研究内容•10
1.6.1研究意义•••10
1.6.2 研究内容•••10
1.7 合成思路••10
1.7.1合成路线•••10
1.8方案论证•••11
2 实验部分•12
2.1 仪器与试剂12
2.1.1 仪器•••12
2.1.2 试剂•••13
2.2 实验步骤••14
2.2.1 取代甲酰苯胺的制备•14
2.2.1.1间甲基甲酰苯胺的制备•14
2.2.1.2对氯甲酰苯胺的制备•••14
2.2.1.3对甲基甲酰苯胺的制备•14
2.2.2 目标化合物的制备•••15
2.2.2.1 N,N-二乙基间甲基苯甲脒的制备•15
2.2.2.2 N,N-二乙基对氯苯甲脒的制备•••15
2.2.2.3 N,N-二乙基对甲基苯甲脒的制备•16
3. 结果与讨论•17
3.1 关于目标化合物的合成••17 无催化熔融法合成脒类化合物研究:http://www.youerw.com/huaxue/lunwen_33455.html