| 吡虫啉生产过程中吗啉精馏副产物的核磁共振分析 |
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| 引用本文： | 张奉民,余华光.吡虫啉生产过程中吗啉精馏副产物的核磁共振分析[J].波谱学杂志,2014,31(3):364-371. |
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| 作者姓名： | 张奉民 余华光 |
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| 作者单位： | 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 |
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| 基金项目： | 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) |
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| 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.
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| 关 键 词： | 核磁共振(NMR) 结构分析 定量 扩散排序谱 吡虫啉 |
| 收稿时间： | 2014-01-18 |
NMR Analysis of By-Products in Imidacloprid Production |
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| ZHANG Feng-min,YU Hua-guang.NMR Analysis of By-Products in Imidacloprid Production[J].Chinese Journal of Magnetic Resonance,2014,31(3):364-371. |
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| Authors: | ZHANG Feng-min YU Hua-guang |
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| Institution: | 1. Testing Center, Yangzhou University, Yangzhou 225009, China;
2. College of Physics Science and Technology, Yangzhou University, Yangzhou 225002, China |
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| 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. |
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| Keywords: | NMR structure analysis quantification DOSY imidacloprid |
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