波谱学杂志
波譜學雜誌
파보학잡지
CHINESE JOURNAL OF MAGNETIC RESONANCE
2014年
3期
364-371
,共8页
核磁共振(NMR)%结构分析%定量%扩散排序谱%吡虫啉
覈磁共振(NMR)%結構分析%定量%擴散排序譜%吡蟲啉
핵자공진(NMR)%결구분석%정량%확산배서보%필충람
NMR%structure analysis%quantification%DOSY%imidacloprid
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.
採用覈磁共振(NMR)技術對吡蟲啉生產過程中嗎啉精餾後的副產物進行瞭定性定量分析.二維擴散排序譜(2D DOSY)錶明該產物由兩種化閤物組成.對樣品的覈磁共振氫譜(1H NMR)、二維擴散排序譜(2D DOSY)、碳譜(13C NMR)、DEPT、氫-氫相關譜(1H-1H COSY)、碳氫相關譜(HSQC)與碳氫遠程相關譜(HMBC)進行瞭解析,對其所有的NMR譜信號進行瞭歸屬,確定樣品所含的兩種主要組份為雙嗎啉和烯胺.最後採用定量13C NMR技術得到瞭該精餾副產物中雙嗎啉和烯胺組成的摩爾比例為1∶4.
채용핵자공진(NMR)기술대필충람생산과정중마람정류후적부산물진행료정성정량분석.이유확산배서보(2D DOSY)표명해산물유량충화합물조성.대양품적핵자공진경보(1H NMR)、이유확산배서보(2D DOSY)、탄보(13C NMR)、DEPT、경-경상관보(1H-1H COSY)、탄경상관보(HSQC)여탄경원정상관보(HMBC)진행료해석,대기소유적NMR보신호진행료귀속,학정양품소함적량충주요조빈위쌍마람화희알.최후채용정량13C NMR기술득도료해정류부산물중쌍마람화희알조성적마이비례위1∶4.
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-dimorpholinopropane and N-(1-propenyl) morpholine. Finally a quantitative 13C NMR method was developed to measure the contents of by-products quantitatively.