杀菌剂氰霜唑的合成新方法  

New Synthesis of Fungicide Cyazofamid

作　　者：王月梅[1] 杨翠凤[1] 林双政[1] 徐泽刚[1] 王伦[1] 刘康云[1] 李秉擘 陈涛[1] 卫天琪 

机构地区：[1]西安近代化学研究所,西安710065

出　　处：《农药》2015年第5期324-326,共3页Agrochemicals

摘　　要：[目的]研究杀菌剂氰霜唑的合成新方法。[方法]以4-甲基苯乙酮为原料,经过氧化、咪唑合环、酯化、氨化、脱水、氯化,最后一步磺酰化合成氰霜唑。重点针对咪唑合环合成步骤进行反应条件优化,得出较佳工艺条件:反应温度85℃,反应时间10 h,溶剂为乙醇,铵盐为(NH4)2CO4,物料比n[2-羰基-2-(4-甲基苯)基乙醛]颐n[(NH4)2CO4]颐n[乙醛酸(50%水溶液)]颐n(三乙胺)为1颐1.5颐3颐5。[结果]路线总收率达37.0%。[结论]该新路线工艺简单,反应条件温和,所有中间体均易提纯和鉴定。[Aims] This paper aims to report the new synthesis of fungicide cyazofamid. [Methods] The compound was synthesized using 4-acetyltoluene as raw materials, through reactions of the oxidation, esterification, ammoniation,dehydration, chlorination and sulfonylation to obtain cyazofamid. And the paper mainly discussed the optimum process conditions for synthesizing substituted imidazole ring： reaction temperature is 85 ℃, reaction time is 10 hours, ethanol as the solvent and n[2-oxo-2-（p- tolyl）acetaldehyde]：n[（NH4）2CO4]：n[glyoxylic acid（50% water solution）]：n（triethylamine）=1：1.5：3：5. [Results] The total yield was 37.0%. [Conclusions] The process is simple, the reaction conditions is mild,All the intermediates are easy to be purified and identified.

关 键 词：氰霜唑 4-甲基苯乙酮 2-羰基-2-(4-甲基苯)基乙醛 乙醛酸 咪唑环 

分 类 号：TQ455[化学工程—农药化工]