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N,N-二甲基-2-(1H-1,2,4-三唑-1-基)乙酰胺的制备

时间:2019-01-11 17:23来源:毕业论文
研究N,N-二甲基-2-(1H-1,2,4-三唑-1-基)乙酰胺的合成工艺。首先以三氮唑和氢氧化钾为原料合成三氮唑钾盐,考察不同带水剂对钾盐成盐的影响;其次以氯乙酸甲酯及二甲胺为原料,经氨解

摘要:本课题主要研究N,N-二甲基-2-(1H-1,2,4-三唑-1-基)乙酰胺的合成工艺。首先以三氮唑和氢氧化钾为原料合成三氮唑钾盐,考察不同带水剂对钾盐成盐的影响;其次以氯乙酸甲酯及二甲胺为原料,经氨解得到反应中间体,同时着重考察反应时间、反应温度及物料配比对中间体收率的影响。最后将钾盐与中间体反应,得到目标产物,考察反应时间、物料配比及溶剂中DMF含量对产物的影响。从而确定了:甲苯为三氮唑钾盐成盐反应良好的带水剂;在5℃下,n[氯乙酸甲酯]:n[二甲胺]=1:1.3,反应4小时为制备2-氯-N,N-二甲基乙酰胺的优化条件;以及,制备目标产物的优化条件:n[2-氯-N,N-二甲基乙酰胺]:n[三氮唑钾盐]=1:1.1,在78℃下反应4小时。并且使用IR对产物进行表征。最终N,N-二甲基-2-(1H-1,2,4-三唑-1-基)乙酰胺的收率可达92.18%。 32584
毕业论文关键词:三氮唑;2-氯-N,N-二甲基乙酰胺;N,N-二甲基-2-(1H-1,2,4-三唑-1-基)乙酰胺;制备
 The Synthesis of  N,N-dimethyl-2-(1H-1,2,4-triazol-1-yl) acetamide
Abstract:1,2,4-Triazole potassium salt was prepared from 1,2,4-triazole and potassium,and investigate the effects of the water-carrying agent on preparation of 1,2,4-triazole potassium salt.Chloral acetic acid methyl ester and Dimethylamine in ethanol solution was prepared as raw materials 2-chloro-N,N-dimethylacetamide. Focus on effects of reaction temperature, reaction time, molar ratio of materials for the purpose of the product yield . At last, potassium salt and 2-chloro-N,N- dimethylacetamide as raw materials to prepare N,N-dimethyl-2- (1 H-1,2,4-triazol- 1- yl) acetamide.The effects of reaction time, molar ratio of materials and the concen- tration of DMF in the solvent on preparation of final product were investigated.The results as follows:toluene is a great water-carrying agent on preparation of 1,2,4- triazole potassium salt.The 2-chloro-N,N- dimethylacetamide conditions as:reaction temperature around 5℃, reaction time 4h, n [Chloral acetic acid methyl ester]: n[Dimethylamine]= 1:1.3. .The optimal reaction conditions as:reaction temperature around 78 ℃, reaction time 4 h , n(2-chloro-N,N- dimethylacetamide):n(1,2,4- Triazole potassium salt)=1:1.1.The yield of N,N-dimethyl-2- (1 H-1,2,4-triazol-1-yl) acetamide was 92.18 %,the product was characterized by IR analysis.

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Keywords:1,2,4-triazole;2-chloro-N,N-dimethylacetamide;N,N-dimethyl-2- (1 H-1,2,4-triazol-1-yl) acetamide;prepare
目 录
1 前言    1
1.1农药概述    1
1.1.1农药的定义    1
1.1.2农药的分类    2
1.1.3我国农药发展简况    2
1.1.4开发新农药的特点及方向    3
1.2文献综述    6
1.2.1 酰胺类农药    6
1.2.2三唑类除草剂    9
1.3本文研究的内容    11
2 实验部分    14
2.1 实验仪器设备与试剂    14
2.1.1 实验仪器与设备    14
2.2 合成方法    15
2.2.1三氮唑钾盐的制备:    15
2.2.2 2-氯-N,N-二甲基乙酰胺的制备    16
2.2.3 N,N-二甲基-2-(1H-1,2,4-三唑-1-基)乙酰胺的制备    16
2.2.3 N,N-二甲基-2-(1H-1,2,4-三唑-1-基)乙酰胺的提纯    16
3 结果与讨论    18
3.1带水剂对三氮唑钾盐制备反应的影响    18
3.2 不同的反应条件对2-氯-N,N-二甲基乙酰胺收率的影响    18
3.2 .1反应时间对2-氯-N,N-二甲基乙酰胺收率的影响    18
3.2.2 反应温度对2-氯-N,N-二甲基乙酰胺收率的影响    19
3.2.3物料摩尔比对2-氯-N,N-二甲基乙酰胺收率的影响    21 N,N-二甲基-2-(1H-1,2,4-三唑-1-基)乙酰胺的制备:http://www.lwfree.cn/huaxue/20190111/29250.html
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