吡虫啉生产过程中吗啉精馏副产物的核磁共振分析

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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Bibliographic Details
Published in波谱学杂志 Vol. 31; no. 3; pp. 364 - 371
Main Author 张奉民 余华光
Format Journal Article
LanguageChinese
Published 扬州大学 测试中心,江苏 扬州,225009%扬州大学 物理科学与技术学院,江苏 扬州,225002 2014
Subjects
吡虫啉
定量
扩散排序谱
核磁共振（NMR）
结构分析
DOSY
NMR
吡虫啉
quantification
扩散排序谱
structure analysis
核磁共振(NMR)
结构分析
定量
imidacloprid
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ISSN1000-4556

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Summary: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.
Bibliography:NMR; structure analysis; quantification; DOSY; imidacloprid
ZHANG Feng-min, YU Hua-guang （1. Testing Center, Yangzhou University, Yangzhou 225009, China; 2. College of Physics Science and Technology, Yangzhou University, Yangzhou 225002, China）
42-1180/04
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 13 C 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-dimorpholinopropane and N-（1-propenyl） morpholine. Finally a quantitative 13 C NMR method was developed to measure the contents of by-products quantitatively.
ISSN:1000-4556