Structure and dynamics of the branched polysaccharide scleroglucan in dilute solutions studied by 1D and 2D NMR spectroscopy

Chitosan derivatives are obtained by reaction of chitosan with a low degree of acetylation and levulinic acid under different experimental conditions. The chemical structure of the different derivatives obtained is determined using 1H and 13C NMR spectroscopies. The intrinsic viscosity is used to follow the molecular weight evolution. Finally, conditions are described in which water-soluble N-carboxybutylchitosan is obtained. In particular, the time of the reduction step and the ratio between reagents are investigated. Under mild conditions and short times of reduction there is a very low degree of substitution and only the monocarboxybutylchitosan is formed. The dicarboxylated form is never observed. The cyclic derivative (5-methylpyrrolidinone chitosan) is obtained when the reducing agent is added slowly to the reactants.