Abstract
TEMPO (2,2,6,6-tetramethylpiperidine-1-oxyl)-mediated oxidation of methyl α-<sc>d</sc>-mannopyranoside with sodium hypochlorite gave sodium (methyl α-<sc>d</sc>-mannopyranosid)uronate, which was obtained as a crystalline monohydrate in ~70% yield without chromatography. Its purity was proved by NMR spectroscopy, a newly developed HPLC method, combustion analysis, and X-ray crystallography. The crystal structure, solved from synchrotron diffraction data in space group <i>P</i>2<sub>1</sub>2<sub>1</sub>2<sub>1</sub>, revealed that the packing of the uronate molecules is connected by an extensive network of hydrogen bonds, and that the Na<sup>+</sup> ion is coordinated by six oxygen ligands from one water and three surrounding sugar molecules.
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