Proton decoupled and undecoupled 13C n.m.r. spectra have been measured on a number of hexopyranoses. The direct coupling constants between the anomeric carbon atoms and protons(lJ[l3C-H (1 )]) were found to be ca. 160 in the P-anomers and ca. 170 Hz in the a-anomers : the difference of ca. 10 Hz between pairs of anomers was found in almost all cases. Chemical shifts and l J ( 1 3 C H ) values of the other carbon atoms in the pyranose rings were also measured.

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I. Introduction and Scope 4589 II. NMR Methods for Structural Determination 4591 A. Carbohydrate Structural Elements and Classical NMR Methods 4591 1. Number of Sugar Residues 4592 2. Constituent Monosaccharides 4592 3. Anomeric Configuration 4593 4. Linkage and Sequence 4594 5. Position of Appended Groups 4594 6. Classical NMR Methods 4594 B. New NMR Methods 4596 C. Computer-Assisted Structural Analysis 4598 D. NMR Spectroscopy of Mixtures 4599 III. Large and Unusual Oligosaccharides 4600 IV. Polysaccharides 4603 V. NMR Analysis of Small Sample Amounts 4604 A. NMR Probes and Sample Tubes 4605 B. Examples of Structural Analysis with Small Sample Amounts 4606 VI. Conclusions 4610 VII. Acknowledgments 4610 VIII. References 4610 † This paper is dedicated to the late Professor R. U. Lemieux in memory of an always exiting and stimulating collaboration on structural studies of oligosaccharides.Jens Ø. Duus received his M.Sc. degree in Chemical Engineering from the Technical University of Denmark in 1989. Following this, he continued his graduate study with Professor Klaus Bock at the Carlsberg Laboratory and was granted his Ph.D. degree from the Technical University of Denmark in 1993. During his graduate study he was twice a Visiting Scientist at Dupont Experimental Station in Wilmington, DE working with Dr. S. Sabesan. From 1993 to 1994 he was a Research Fellow in Chemistry at the Beckman Institute at the California Institute of Technology working with Professor Harry B. Gray. After returning to the Carlsberg Laboratory, he was appointed Senior Scientist. His main fields of research are structure and dynamics of biomolecules with emphasis on carbohydrates using NMR and fluroescence.

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