异噁唑草酮的绿色合成工艺  

Green synthesis process of isoxaflutole

作　　者：许遥 陈佳易 XU Yao;CHEN Jiayi(Shangyu Nutrichem Co.,Ltd.,Shaoxing 312300,Zhejiang,China)

机构地区：[1]上虞颖泰精细化工有限公司,浙江绍兴312300

出　　处：《世界农药》2024年第7期28-32,36,共6页World Pesticide

摘　　要：为探索异噁唑草酮绿色合成工艺,采用甲苯作为单一溶剂进行回收套用,以2-硝基-4-三氟甲基苯腈为起始原料,经甲硫基化、氧化、加成缩合水解、烯醇化和环合共6步反应合成了异噁唑草酮,并优化了各步反应条件。优化条件下,甲硫基化收率96.6%、氧化收率97.9%、与环丙基甲基酮加成缩合水解收率95.0%、6步反应总收率78.5%,产品纯度98.0%。该工艺原料廉价易得,操作简单,中间体无需分离纯化,适合工业化生产。To explore the green synthesis process of isoxaflutole,toluene was used as a single solvent for recycling and reusing.Starting from 2-nitro-4-(trifluoromethyl)benzonitrile,isoxaflutole was synthesized through six steps of methylthiolation,oxidation,addition-condensation,hydrolyzation,enolization and cyclization.The reaction conditions for each step were optimized.Under the optimized conditions,the yields of methylthiolation,oxidation,and addition-condensation-hydrolyzation with cyclopropyl methyl ketone were 96.6%,97.9%and 95.0%.The total yield of the six-step reaction was 78.5%,and the product purity was 98.0%.This process uses inexpensive and readily available raw materials,has simple operation,circumvents separation and purification of intermediates,and is suitable for industrial production.

关 键 词：异噁唑草酮 除草剂 合成 工业化 

分 类 号：TQ457.2[化学工程—农药化工]