吡唑解草酯的合成工艺  

The Synthesis of Mefenpyr-diethy

作　　者：范龙涛 郭庆春 徐莉 王萌斐 晁建平[1] 彭效明[1] 居瑞军[1] FAN Long-tao;GUO Qing-chun;XU Li;WANG Meng-fei;CHAO Jian-ping;PENG Xiao-ming;JU Rui-jun(School of Chemical Engineering,Beijing Institute of Petrochemical Technology,Beijing 102617,China;Hebei Lansheng Biotech Co.,Ltd.,Jinzhou 052260,Hebei,China)

机构地区：[1]北京石油化工学院化学工程学院,北京102617 [2]河北兰升生物科技有限公司,河北晋州052260

出　　处：《农药》2020年第5期328-331,346,共5页Agrochemicals

基　　金：国家自然科学基金资助项目(81703453);北京市大兴区科技发展计划项目(KT201806402)。

摘　　要：[目的]以2,4-二氯苯胺为原料开发吡唑解草酯生产工艺。[方法]改进现存吡唑解草酯的合成工艺,探索生产工艺的合成条件。通过单因素试验探讨了硫酸浓度、反应温度、pH值、物料比、结晶溶剂等因素对反应的影响,确定合成吡唑解草酯的工艺条件。[结果]产品收率96.8%,纯度99.2%,终产品经核磁表征。[结论]工艺过程处理简洁,无固体生成,有利于产品实现连续化生产。[Aims]This study aims to develop a production process of pyrazolofen by using 2,4-dichloroaniline as the raw material.[Methods]The methods are to improve the existing synthetic process of pyrazolidin and to explore the synthetic conditions of production process.The effects of sulfuric acid concentration,reaction temperature,pH,material ratio,crystallization solvent and other factors on the reaction were explored through single-factor experiments,and the continuous process for the synthesis of pymepyramine were determined.[Results]The yield of the product was 96.8%,and the purity was 99.2%.The final product was characterized by NMR and mass spectrometry.[Conclusions]The process is simple in processing and no solids are generated,which is conducive to continuous production of products.

关 键 词：2 4-二氯苯胺 重氮化 2-氯-2-(2 4-二氯苯腙基)-乙醛酸乙酯 环合反应 吡唑解草酯 

分 类 号：TQ460.3[化学工程—制药化工]