摘要:以氯乙酸甲酯为原料,在无水碳酸钾存在下,N,N-二甲基甲酰胺(DMF)为溶剂,与不同的酚类化合物反应,得到中间体芳氧乙酸甲酯(Ⅰ);进而,中间体(Ⅰ)与不同的胺反应,得到产物芳氧乙酰胺类化合物。本文还着重考察了反应温度、反应时间、物料投料比对芳氧乙酸甲酯及第二步产物N -甲基-2-(苯氧基)乙酰胺、N,N-二甲基-2-(苯氧基)乙酰胺收率的影响,从而确定了合成工艺条件为:反应温度80℃,反应时间4.0 h,物料投料比n(氯乙酸甲酯)n(苯酚)=1.0:1.2。在此条件下,第一步产物芳氧乙酸甲酯的收率达75%以上。反应温度:40℃,反应时间4.0 h ,物料投料比n(苯氧乙酸甲酯):n(二甲胺)=1.0:2.0。第二步产物收率N -甲基-2-(苯氧基)乙酰胺(Ⅱ)收率达70%以上;反应温度:30℃,反应时间4.0h,物料投料比n(苯氧乙酸甲酯): n(甲胺)=1.0:2.5。第二步产物收率N,N-二甲基-2-(苯氧基)乙酰胺(Ⅲ) 收率达70%以上。从中选出合适条件又合成了N,N-二甲基-2-(4-氯苯氧基)乙酰胺。33076
毕业论文关键词: 氯乙酸甲酯;苯酚;对氯苯酚;二甲胺;甲胺;N-甲基-2-(苯氧基)乙酰胺
Synthesis of acetyl amine compound
Abstract: Chloroacetic acid methyl ester as the starting material, anhydrous potassium carbonate in the presence of a catalyst, N, N- dimethylformamide (DMF) as solvent, with various phenolic compounds, intermediates phenoxyacetate (Ⅰ); Furthermore, intermediate (Ⅰ) is reacted with various amines to give the product aryloxy acetamides. Also paper also examines the reaction temperature, reaction time, material feed ratio on the first step of the product (Ⅰ) and the yield of the second step, in order to determine the conditions were as follows: reaction temperature 80 ℃, reaction time 4.0h, material feed ratio of n (acid methyl ester): n (phenol) = 1.0: 1.2. Under this condition, the first step in the product (Ⅰ) the yield of 75% or more. Reaction temperature: 40 ℃, reaction time 4.0h, material feed ratio n (phenoxyacetate): n (dimethylamine) = 1.0: 2.0. Step product yields (Ⅱ) yield of over 70%; reaction temperature: 30 ℃, reaction time 4.0h, material feed ratio n (phenoxyacetate): n (trimethylamine) = 1.0: 2.5. Step product yields (Ⅲ) yield of over 70%.
Keywords: acid ester; phenol; p-chlorophenol; dimethlamine; trimethylamine; N-methyl-2-(phenoxy) acetamide
目录
1 前言 1
1.1 课题的目的和意义 1
1.2 国内外研究现状与水平 2
1.3 我国农药行业存在的问题 3
1.3.1 药剂自身的毒性问题 3
1.3.2 “三废”和杂质问题 3
1.3.3 光学体合成问题 3
1.4 文献查阅、调研情况 4
1.4.1 乙酰胺类的性质 4
1.4.2 乙酰胺类的分类 4
1.5 乙酰胺类的制备方法 7
1.5.1 方法一 7
1.5.2 方法二 7
1.5.3 方法三 7
1.5.4 研究内容 8
2 实验部分 9
2.1 实验的仪器和试剂 9
2.1.1 实验仪器 9
2.1.2 试剂及其物性常数 10
2.2产物的制备 10
2.2.1 苯氧乙酸甲酯的制备 10
2.2.2 N,N-二甲基-2-(苯氧基)乙酰胺的制备 10
2.2.3 N -甲基-2-(苯氧基)乙酰胺的制备 11
2.2.4 2-(4-氯苯氧基)乙酸甲酯的制备 11
2.2.5 N,N-二甲基-2-(4-氯苯氧基)乙酰胺的制备 11
3 结果与讨论 12
3.1 苯氧乙酸甲酯的制备 12 乙酰胺类化合物的合成+文献综述:http://www.751com.cn/huaxue/lunwen_29942.html