“一锅三步法”合成2,4-二氯苯胺  

One-pot three-step method for the synthesis of 2,4-dichloroaniline

作　　者：王奥 王萌斐 王红平 杨红瑾 彭效明[1] 严晓强 晁建平[1] WANG Ao;WANG Meng-fei;WANG Hong-ping;YANG Hong-jin;PENG Xiao-ming;YAN Xiao-qiang;CHAO Jian-ping(College of New Materials and Chemical Engineering,Beijing Institute of Petrochemical Technology,Beijing 102617,China;Beijing Tianhong Tianda Medicine Co.,Ltd.,Beijing 102629,China)

机构地区：[1]北京石油化工学院新材料与化工学院,北京102617 [2]北京天虹天达医药科技股份有限公司,北京102629

出　　处：《农药》2022年第11期795-797,共3页Agrochemicals

基　　金：国家自然科学基金资助项目(81703453);北京石油化工学院校内学科平台建设项目(2019XK006)。

摘　　要：[目的]筛选出2,4-二氯苯胺的最佳合成工艺条件,降低生产成本、减少环境污染。[方法]以2,4-二氯苯酚和2-氯乙酰胺为原料,在DMSO中,通过“一锅三步法”(即串联O-烷基化、Smiles重排反应、水解反应)合成了2,4-二氯苯胺,并对其合成条件和分离工艺进行优化。[结果]最优反应条件下,产品收率为68.3%,纯度为99.1%。[结论]该实验优化了2,4-二氯苯胺的合成及提纯工艺,以一种操作更简单、安全、廉价的方法合成了2,4-二氯苯胺。[Aims] This study aims to screen out the optimal synthesis process of 2,4-dichloroaniline, with low cost and low environmental pollution. [Methods] Using 2,4-dichlorophenol and 2-chloroacetamide as the raw materials, DMSO as solvent, 2,4-dichloroaniline was synthesized by a “one-pot three-step method”(ie, tandem O-alkylation, Smiles rearrangement, and hydrolysis), its synthesis conditions and separation process were optimized as well. [Results] Under the optimal reaction conditions, the yield was 68.3% and the product purity was 99.1%. [Conclusions] The synthesis and purification process of 2,4-dichloroaniline was optimized in this experiment, and a simpler, safer and cheaper method for synthesizing 2,4-dichloroaniline was provided.

关 键 词：2 4-二氯苯酚 Smiles重排 2 4-二氯苯胺 

分 类 号：TQ460.3[化学工程—制药化工]