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摘要：以氯乙酸甲酯和4-氯苯酚为原料，N,N-二甲基甲酰胺(DMF)为有机溶剂，在无水碳酸钾的存在下，反应数小时，制备2-(4-氯苯氧基)乙酸甲酯。然后，由2-(4-氯苯氧基)乙酸甲酯和二甲胺在DMF溶液中反应数小时，制备了中间产物化合物N,N-二甲基-2-(4-氯苯氧基)乙酰胺。再经硫酰氯氯化，得到目的产物N,N-二甲基-2-(2,4-二氯苯氧基)乙酰胺。着重考察了反应温度、反应时间、物料投料摩尔比对中间产物2-(4-氯苯氧基)乙酸甲酯、N,N-二甲基-2-(4-氯苯氧基)乙酰胺及目的产物N,N-二甲基-2-(2,4-二氯苯氧基)乙酰胺收率的影响，从而确定了2-(4-氯苯氧基)乙酸甲酯的合成工艺条件为反应温度80℃,反应时间为5小时,投料比n(4-氯苯酚)：n(氯乙酸甲酯)=1:1.3，DMF为反应溶剂;N,N-二甲基-2-(4-氯苯氧基)乙酰胺的合成工艺条件为反应温度为50℃,反应时间为4小时,投料比n[2-(4-氯苯氧基)乙酸甲酯]：n(二甲胺)=1:3，DMF为反应溶剂;及N,N-二甲基-2-(2,4-二氯苯氧基)乙酰胺的合成工艺条件为：反应温度40℃，反应时间4h，n[N-甲基-2-(4-氯苯氧基)乙酰胺]：n(硫酰氯)= 1.0:1.5，甲酸为反应溶剂。在此优化条件下，中间产物2-(4-氯苯氧基)乙酸甲酯的产率达80%;中间产物N,N-二甲基-2-(4-氯苯氧基)乙酰胺的收率达78%以上;目的产物N,N-二甲基-2-(2,4-二氯苯氧基)乙酰胺的收率达70%以上。化合物的结构经元素、IR、1HNMR分析进行了表征。31501
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毕业论文关键词： 2-(4-氯苯氧基)乙酸甲酯；N,N-二甲基-2-(4-氯苯氧基)乙酰胺；N,N-二甲基-2-(2,4-二氯苯氧基)乙酰胺；氯化
Synthesis of N,N-dimethyl-2-(2,4-bichlorophenoxy)
acetamide
Abstract: With methyl chloroacetate and 4 - chlorine phenol as raw materials, N,N - dimethyl formamide (DMF) as organic solvent, in the presence of anhydrous potassium carbonate, reaction for several hours, the preparation of 2 - (4 - chlorobenzene oxygen radicals) methyl acetate. Then, by 2 - (4 - chlorobenzene oxygen radicals) methyl acetate and dimethylamine in DMF solution reaction for several hours, the preparation of the intermediate compounds of N,N - dimethyl - 2 - (4 - chlorobenzene oxygen radicals) acetamide. Then through sulfuryl chloride, chloride to get objective product N,N - dimethyl - 2 - (2,4 - dichlorobenzene oxygen radicals) acetamide. Focuses on the reaction temperature, reaction time, material feeding molar ratio on the intermediate 2 - (4 - chlorobenzene oxygen radicals) methyl acetate, N,N - dimethyl - 2 - (4 - chlorobenzene oxygen radicals) acetamide and objective product N,N - dimethyl - 2 - (2,4 - dichlorobenzene oxygen radicals) influence the yield of acetamide, and thus determine the 2 - (4 - chlorobenzene oxygen radicals) methyl acetate synthesis process conditions for the reaction temperature is 80 ℃, reaction time is 4 hours, weight ratio of n (4 - chlorine phenol) : n(methyl chloroacetate) = 1:1. 3, DMF as solvent; N,N - dimethyl - 2 - (4 - chlorobenzene oxygen radicals) acetamide synthetic process conditions for the reaction temperature is 50 ℃, the reaction time is 4 hours, weight ratio of n(2 - (4 - chlorobenzene oxygen radicals) methyl acetate) : n (dimethylamine) = 1:3, DMF as solvent. And N, N - dimethyl - 2 - (2, 4 - dichlorobenzene oxygen radicals) acetamide synthetic technology conditions as follows: reaction temperature is 40 ℃, reaction time is 4 h and n (N,N - dimethyl - 2 - (4 - chlorobenzene oxygen radicals) acetamide) : n (sulfuryl chloride) = 1.0:1.5, formic acid as reaction solvent. Under the optimized conditions, the intermediate 2 - (4 - chlorobenzene oxygen radicals) methyl acetate production rate of 80%; Intermediate N, N - dimethyl - 2 - (4 - chlorobenzene oxygen radicals) acetamide yield of above 78%; Objective product N,N - dimethyl - 2 - (2,4 - dichlorobenzene oxygen radicals) acetamide yield of above 70%. The structure of the compound element, characterized by IR, 1 HNMR analysis.
KeyWords：； 2-(4-chlorophenoxy) melthyl acetate ；N,N-dimethyl-2-(2- chlorophenoxy) acetamide； N,N-dimethyl-2-(2,4-bichlorophenoxy) acetamide ；chloroacetate
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