高等学校化学学报

• 研究论文 • 上一篇    

除草剂烯草酮关键中间体的连续化合成工艺

任世伦1,黄城1,陈见爱1,李蜜蜜1,马景瑞2,袁其亮3,谭成侠1   

  1. 1. 浙江工业大学
    2. 上海嘉胜石油化工有限公司
    3. 浙江中欣氟材股份有限公司
  • 收稿日期:2025-07-07 修回日期:2025-07-31 网络首发:2025-08-05 发布日期:2025-08-05
  • 通讯作者: 谭成侠 E-mail:tanchengxia@zjut.edu.cn
  • 基金资助:
    一帆生物科技集团股份有限公司资助项目(KYY-HX-20240994)资助

The continuous synthesis process of key intermediates for the herbicide clethodim

REN Shilun1,HUANG Cheng1,CHEN Jianai1,Li Mimi1,MA Jingrui2,YUAN Qiliang3,TAN Chengxia1   

  1. 1. College of Chemical EngineeringZhejiang University of Technology 2. Shanghai Jiasheng Petrochemical Co..Ltd. 3. Zhejiang Zhongxin Fluorine Material Co..Ltd.

  • Received:2025-07-07 Revised:2025-07-31 Online First:2025-08-05 Published:2025-08-05
  • Contact: TAN Chengxia E-mail:tanchengxia@zjut.edu.cn
  • Supported by:
    Supported by the Yifan Bio-Tech Group Co..Ltd. (Grant No. KYY-HX-20240994)

摘要: 烯草酮因其高效、低毒、杀草谱广、施用期长以及对后茬作物安全等特点,现已成为环己烯酮类除草剂的代表性品种. 5-[2-(乙硫基)-丙基]-2-丙酰基-3-羟基-2-环己烯-1-酮(简称精三酮)作为烯草酮的关键中间体,其传统间歇式合成工艺存在反应效率低、能耗较大等问题. 本研究基于微通道连续流技术,开发了关键步骤的连续化合成工艺. 通过优化环合与水解步骤,反应时间从90 min缩短至4.8 min,产物收率达65.2%,纯度95.2%. 该工艺显著提升了反应效率与产物质量,为烯草酮的工业化生产提供了新方法.

关键词: 除草剂, 烯草酮, 微通道连续流技术, 合成工艺

Abstract: Clethodim, known for its high efficacy, low toxicity, broad herbicidal spectrum, extended application window, and safety to subsequent crops, has become a representative cyclohexenone herbicide.?5-[2-(Ethylthio)propyl]-2-propionyl-3-hydroxy-2-cyclohexen-1-one?(abbreviated as?Jing-Santong), a key intermediate of clethodim, faces challenges in traditional batch synthesis, such as low reaction efficiency and high energy consumption.This study developed a?continuous-flow microchannel technology?for the critical synthesis steps. By optimizing the?cyclization and hydrolysis processes, the reaction time was reduced from?90 min to 4.8 min, achieving a?65.2% yield?and?95.2% purity. The novel process significantly improves?reaction efficiency?and?product quality, offering a promising approach for the?industrial production of clethodim.

Key words: Herbicide, Clethodim, Microchannel continuous flow technology, Synthesis process

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