Complete 1H and 13C NMR assignment of cellulose oligomer in LiCl/DMSO

Abstract

AbstractHigh-resolution solution-state 1H, 13C, and various 2D nuclear magnetic resonance (NMR) spectra of cellulose were obtained using cellulose oligomer dissolved in LiCl/dimethyl sulfoxide, which enabled the assignment of all 1H and 13C resonances. The observed resonances were classified into four groups of glucose rings, corresponding to internal residue, non-reducing end, and reducing ends with α- and β-anomeric configurations. This assignment included the OH protons, which are difficult to assign in cellulose using other solvent systems. NMR measurements and assignments were performed using different LiCl concentrations because information on the hydroxy protons is important for understanding the interaction between cellulose and the solvent. The resonances from the OH protons shifted downfield with increasing LiCl concentration, suggesting that LiCl was attracted to the hydroxy groups of cellulose in solution. Moreover, the magnitude of the shifts varied depending on the positions of the hydroxy groups, which indicated the regioselectivity of the interaction between LiCl and the cellulose hydroxy groups. Graphical abstract