砜吡草唑不同合成路线中1-甲基-3-三氟甲基-4-羟甲基-5-二氟甲氧基-1H-吡唑的残余比较  

Comparison of residual 1-methyl-3-trifluoromethyl-4-hydroxymethyl-5-difluoromethoxy-1H-pyrazole in different synthetic routes of pyroxasulfone

作　　者：李朝旭 黄琛 王光杰 王淮 马晓静 朱慧霞 肖华 LI Chaoxu;HUANG Chen;WANG Guangjie;WANG Huai;MA Xiaojing;ZHU Huixia;XIAO Hua(School of Food and Biological Engineering,Hefei University of Technology,Hefei 230601,China)

机构地区：[1]合肥工业大学食品与生物工程学院,合肥230601

出　　处：《农药》2024年第12期879-883,共5页Agrochemicals

基　　金：国家自然科学基金项目(21302034);中央高校基本科研业务专项资金资助项目(JZ2019HGTB0058)。

摘　　要：[目的]探讨砜吡草唑不同合成路线中1-甲基-3-三氟甲基-4-羟甲基-5-二氟甲氧基-1H-吡唑中间体(A2)的残余情况。[方法]选择3条合成路线制备砜吡草唑,其中路线1不使用A2,路线2、3使用A2,对来自不同路线的样品进行A2中间体的分析与检测,并推测其来源。[结果]在3条路线中均检测出A2中间体,推测路线1中A2来自于1-甲基-3-三氟甲基-4-羟甲基-5-羟基-1H-吡唑(A1)的二氟甲基化副反应,路线2、3中A2属于未反应完的中间体残余。[结论]在不使用A2中间体路线的样品中也检测出了该中间体,砜吡草唑及相关样品中A2中间体的检出不能证明合成路线使用了该中间体。[Aims]This study aims to investigate the residues of 1-methyl-3-trifluoromethyl-4-hydroxymethyl-5-difluoromethoxy-1H-pyrazole(A2)found in different synthetic routes of pyroxasulfone.[Methods]Pyroxasulfone was synthesized via 3 different routes,among them routes 2 and 3 used intermediate A2,while route 1 did not.The resulting samples were analyzed for the presence of A2,and the potential sources of A2 residues were inferred.[Results]Intermediate A2 was found in all the three synthetic routes.In Route 1,A2 was speculated to be originated from side reaction of difluoromethylation of 4-(hydroxymethyl)-1-methyl-3-(trifluoromethyl)-1H-pyrazol-5-ol.In Routes 2 and 3,A2 was attributed to residual substrates from the synthesis process.[Conclusions]The intermediate A2 is found in samples from routes that do not use it,which suggests that the detection of A2 can′t confirm the use of it in the synthetic pathway of pyroxasulfone.

关 键 词：砜吡草唑 中间体 合成 检测 专利保护 

分 类 号：TQ453.2[化学工程—农药化工]