期刊
MAGNETIC RESONANCE IN CHEMISTRY
卷 45, 期 10, 页码 883-888出版社
JOHN WILEY & SONS LTD
DOI: 10.1002/mrc.2064
关键词
unsymmetrical indirect covariance; C-13-N-15 heteronuclear correlation; H-1-C-13 GHSQC; H-1-C-13 GHMBC; H-1-N-15 IMPEACH-MBC; C-13-N-15 HSQC-IMPEACH; C-13-N-15 HMBC-IMPEACH
Utilization of long-range H-1-N-15 heteronuclear chemical shift correlation has continually grown in importance since the first applications were reported in 1995. More recently, indirect covariance NMR methods have been introduced followed by the development of unsymmetrical indirect covariance processing methods. The latter technique has been shown to allow the calculation of hyphenated 2D NMR data matrices from more readily acquired nonhyphenated 2D NMR spectra. We recently reported the use of unsymmetrical indirect covariance processing to combine H-1-C-13 GHSQC and H-1-N-15 GHMBC long-range spectra to yield a C-13-N-15 HSQC-HMBC chemical shift correlation spectrum that could not be acquired in a reasonable period of time without resorting to N-15-labeled molecules. We now report the unsymmetrical indirect covariance processing of H-1-C-13 GHMBC and H-1-N-15 IMPEACH spectra to afford a C-13-N-15 HMBC-IMPEACH spectrum that has the potential to span as many as six to eight bonds. Correlations for carbon resonances long-range coupled to a protonated carbon in the 1H-13C HMBC spectrum are transferred via the long-range H-1-N-15 coupling pathway in the H-1-N-15 IMPEACH spectrum to afford a much broader range of correlation possibilities in the C-13-N-15 HMBC-IMPEACH correlation spectrum. The indole alkaloid vincamine is used as a model compound to illustrate the application of the method. Copyright 2007 John Wiley & Sons, Ltd.
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