波谱学杂志

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吡虫啉生产过程中吗啉精馏副产物的核磁共振分析

张奉民1,余华光2   

  1. 1. 扬州大学 测试中心,江苏 扬州 225009;2. 扬州大学 物理科学与技术学院,江苏 扬州 225002
  • 收稿日期:2014-01-18 修回日期:2014-07-18 出版日期:2014-09-05 发布日期:2014-09-05
  • 作者简介:张奉民(1978-),男,山东肥城人,助理研究员,研究方向为核磁共振技术开发与应用.电话:0514-87979022. E-mail:fmzhang@yzu.edu.cn;fmzhluck@163.com. *通讯联系人.
  • 基金资助:

    国家自然科学基金资助项目(21005069),江苏省大型科学仪器设备共享服务平台理事会资助项目(BZ201202).

NMR Analysis of By-Products in Imidacloprid Production

ZHANG Feng-min1,YU Hua-guang2   

  1. 1. Testing Center, Yangzhou University, Yangzhou 225009, China;
    2. College of Physics Science and Technology, Yangzhou University, Yangzhou 225002, China
  • Received:2014-01-18 Revised:2014-07-18 Online:2014-09-05 Published:2014-09-05
  • About author:ZHANG Feng-min, Tel: +86-514-87979022, E-mail: fmzhang@yzu.edu.cn.
  • Supported by:

    国家自然科学基金资助项目(21005069),江苏省大型科学仪器设备共享服务平台理事会资助项目(BZ201202).

摘要:

采用核磁共振(NMR)技术对吡虫啉生产过程中吗啉精馏后的副产物进行了定性定量分析.二维扩散排序谱(2D DOSY)表明该产物由两种化合物组成.对样品的核磁共振氢谱(1H NMR)、二维扩散排序谱(2D DOSY)、碳谱(13C NMR)、DEPT、氢-氢相关谱(1H-1H COSY)、碳氢相关谱(HSQC)与碳氢远程相关谱(HMBC)进行了解析,对其所有的NMR 谱信号进行了归属,确定样品所含的两种主要组份为双吗啉和烯胺.最后采用定量13C NMR 技术得到了该精馏副产物中双吗啉和烯胺组成的摩尔比例为1∶4.

关键词: 核磁共振(NMR), 结构分析, 定量, 扩散排序谱, 吡虫啉

Abstract:

In this paper, qualitative and quantitative NMR techniques were used to analyze samples obtained from imidacloprid production. Two-dimensional DOSY spectra demonstrated the samples contained two by-products. One-dimensional (i.e., 1H and 13C NMR and DEPT) and two-dimensional (i.e., 1H-1H COSY, HSQC and HMBC) NMR techniques were used to assign the chemical shifts of the by-products, which were finally determined to be 1,1-imorpholinopropane and N-(1-propenyl) morpholine. Finally a quantitative 13C NMR method was developed to measure the contents of by-products quantitatively.

Key words: NMR, structure analysis, quantification, DOSY, imidacloprid

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