农药学学报2024，Vol.26Issue(1)：61-68,8.DOI:10.16801/j.issn.1008-7303.2023.0099
丙硫菌唑合成工艺中副产物形成分析
Analysis of by-products formation in the synthetic processes of prothioconazole
摘要
Abstract
Some side reactions in the synthetic processes of prothioconazole led to by-products.They negatively affect the yield and quality of prothioconazole.Three different synthetic processes were investigated.Four by-products,including 2-(1-chlorocyclopropyl)-1-(2-chlorophenyl)-3-(4H-1,2,4-triazol-4-yl)propan-2-ol(7),6-(2-chlorobenzyl)-6-(1-chlorocyclopropyl)-5,6-dihydro-4H-1,3,4-oxadiazine-4-carbothioamide(8),dimer-prothioconazole(9)and 2-(2-chlorobenzyl)-2-((5-thioxo-4,5-dihydro-1,2,4-triazol-1-yl)methyl)cyclobutanone(10),were synthesized and characterized by 1H NMR,13C NMR,ESI-MS or X-Ray diffraction.Among them,the by-product 8 was first discovered during the synthesis of prothioconazole by substituting hydrazine-acetone.The study revealed the mechanism of generation of the four by-products in different processes.The results provided an important guide for the selection and control of the synthetic process of prothioconazole and product quality improvement.关键词
丙硫菌唑/合成工艺/副产物/结构表征Key words
prothioconazole/synthetic processes/by-products/structure characterization分类
化学化工引用本文复制引用
闫景铭,王夏菲,程绎南,张蒙萌,马艺超,王利民,李洪连..丙硫菌唑合成工艺中副产物形成分析[J].农药学学报,2024,26(1):61-68,8.基金项目
河南省重大公益性科研专项经费资助(201300111600). Supported by Major Public Welfare Scientific Research Project of Henan Province(No.201300111600). （201300111600）
