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Measurement of one-bond proton-carbon coupling constants of saccharides

✍ Scribed by Stanislava Uhrínova; Dušan Uhrían; Tibor Liptaj; Juraj Bella; Ján Hirsch

Publisher
John Wiley and Sons
Year
1991
Tongue
English
Weight
815 KB
Volume
29
Category
Article
ISSN
0749-1581

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✦ Synopsis

Abstract

Several NMR experiments, one proton and several carbon detected, were used for the determination of ^1^J(C,H) values in saccharides. Couplings of anomeric carbons were measured from the ^13^C satellites in ^1^H NMR spectra. The simultaneous application of several purging schemes resulted in a very good suppression of the proton signals from ^12^C molecules. ^1^J(C,H) values of all saccharides were determined by 2D J‐resolved spectroscopy using an INEPT‐type pulse sequence with a BIRD pulse for the suppression of ^n^J(C,H) and folding in F~1~. Rules for the calculation of the correct values of ^1^J(C,H) from the observed reduced splittings are proposed. ^1^J(C,H) values were also obtained from a set of J‐modulated one‐dimensional ^13^C spectra. A procedure for the determination of ^1^J(C,H) values from only two one‐dimensional experiments is proposed. Mannose derivatives (mono‐ and poly‐saccharides) were used to test and compare the individual methods. Differences in ^1^J(C,H) values for C‐2 and C‐3 were used for the chemical shift assignment of these carbons.

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