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13C取代碳水化合物的同位素编辑一维和二维核磁共振光谱

Isotope-edited 1D and 2D n.m.r. spectroscopy of 13C-substituted carbohydrates.

作者信息

Wu J, Serianni A S

机构信息

Department of Chemistry and Biochemistry, University of Notre Dame, IN 46556.

出版信息

Carbohydr Res. 1992 Mar 30;226(2):209-18. doi: 10.1016/0008-6215(92)84068-4.

DOI:10.1016/0008-6215(92)84068-4
PMID:1617685
Abstract

Three isotope-edited n.m.r. methods have been applied to selectively 13C-substituted monosaccharides and nucleosides to simplify their spectra and/or measure 1H-1H, 13C-1H, or 13H-13C spin-couplings detected via the labeled site. 1D INADEQUATE spectra allowed the selective detection of the natural-abundance carbons that are spin-coupled to the labeled carbon, and adjustment of the mixing time permitted further discrimination between one-bond and longer-range 13C-13C coupling pathways. Geminal and vicinal 13C-1H coupling constants were determined from the analysis of 1H-1H COSY cross-peaks for those protons coupled to the labeled carbon. Long-range 13C-(HETCOR) and 1H-detected (HMBC) 13C-1H chemical-shift correlation spectra permitted the selective observation of those protons coupled to the labeled site, and JH,H values were measured from data projections. The implications of these methods for structural studies of more complex systems is briefly discussed.

摘要

三种同位素编辑的核磁共振方法已应用于选择性13C取代的单糖和核苷,以简化它们的光谱和/或测量通过标记位点检测到的1H-1H、13C-1H或13C-13C自旋耦合。一维INADEQUATE光谱允许选择性检测与标记碳自旋耦合的天然丰度碳,并且通过调整混合时间可以进一步区分一键和长程13C-13C耦合路径。从与标记碳耦合的那些质子的1H-1H COSY交叉峰分析中确定偕偶和邻位13C-1H耦合常数。远程13C-(HETCOR)和1H检测(HMBC)13C-1H化学位移相关光谱允许选择性观察与标记位点耦合的那些质子,并从数据投影中测量JH,H值。简要讨论了这些方法对更复杂系统结构研究的意义。

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