2-氯-5-氯甲基噻唑纯化工艺的杂质分析  

Analytical Investigations to Support Process Impurity Mapping:2-Chloro-5-chloromethylthiazole Purification Process

作　　者：丛云波 蒋爱忠 左伯军 CACHAT Dorian BUCHARD Sarah CIOBANU Edith CONG Yun-bo;JIANG Ai-zhong;ZUO Bo-jun;CACHAT Dorian;BUCHARD Sarah;CIOBANU Edith(Key Laboratory for Chemical Pesticide of Shandong Province,Shandong Academy of Pesticide Sciences,Jinan 250033,China;Process Technology and Analytics,Syngenta Crop Protection,Monthey 1870,Switzerland)

机构地区：[1]山东省农药科学研究院山东省化学农药重点实验室,济南250033 [2]先正达植物保护公司工艺技术与分析部,瑞士蒙泰1870

出　　处：《农药》2020年第8期576-578,581,共4页Agrochemicals

基　　金：山东省农业科学院农业科技创新工程产业团队(CXGC2016B12)。

摘　　要：[目的]2-氯-5-氯甲基噻唑是影响噻虫嗪含量的关键中间体,试验对其纯化工艺的杂质分析策略进行介绍。[方法]利用高效液相色谱或气相色谱、液相色谱或气相色谱与质谱联用、制备或快速制备液相色谱以及核磁等技术,促进工艺团队对特定工艺杂质形成的理解。[结果]成功对CCT纯化工艺中的7个杂质进行定性分析。[结论]这些发现有助于理解杂质EXC9164的形成机制,进而有助于深入理解CCT的合成工艺。[Aims]2-Chloro-5-chloromethylthiazole is a key intermediate that affects the purity of thiamethoxam.This study aims to describe an analytical strategy deployed to support the process impurity of 2-chloro-5-chloromethylthiazole purification process.[Methods]Techniques such as high-performance liquid chromatography(HPLC)or gas chromatography(GC),liquid or gas chromatography coupled with mass spectroscopy(LC-MS,GC-MS),preparative or flash liquid chromatography and nuclear magnetic resonance(NMR)were employed to support process teams in understanding the formation of specific process impurities.[Results]The seven impurities in the CCT purification process were qualitatively analyzed successfully.[Conclusions]These findings are of great help in understanding the mechanism of formation of EXC9164 and consequently in increasing CCT process knowledge.

关 键 词：工艺杂质 2-氯-5-氯甲基噻唑 噻虫嗪 

分 类 号：TQ450.7[化学工程—农药化工]