New and old NMR experiments for the resonance assignment of complex oligosaccharides—application to a cyclodextrin derivative

✍ Scribed by B. Plainchont; A. Martinez; S. Tisse; J.-P. Bouillon; F. Pilard; J.-M. Wieruszeski; G. Lippens; D. Jeannerat; J.-M. Nuzillard

• Publisher: John Wiley and Sons
• Year: 2011
• Tongue: English
• Weight: 448 KB
• Volume: 49
• Category: Article
• ISSN: 0749-1581
• DOI: 10.1002/mrc.2828

✦ Synopsis

The complete assignment of the ^1^H and ^13^C sugar resonances in mono‐3,6‐anhydro‐heptakis(2,3‐O‐methyl)‐hexakis(6‐O‐methyl)‐β‐cyclodextrin, an asymmetrically functionalized β‐cyclodextrin, was carried out by means of 2D NMR experiments. The TOCSY and the homonuclear multiple relay COSY spectra provided most of the ^1^H assignments. The multiplicity edited HSQC and a set of F~1~ selective HSQC‐TOCSY and multiple relay HSQC‐COSY spectra gave access to most of the ^13^C chemical shifts. The latter were fully and accurately determined by means of a pair of complementary, highly folded HSQC‐TOCSY spectra. The TOCSY‐ROESY and ROESY‐TOCSY spectra yielded the sequential assignment of the sugar units. A high resolution F~1~ selective F~1~ decoupled version of the TOCSY‐ROESY experiment was recorded. Copyright © 2011 John Wiley & Sons, Ltd.