Abstract Chemical methods are described for preparing unenriched and [1-13 C]-enriched 5- deoxy-and 5-O-methyl-pentoses in the D or l configuration. The 1 Hn. mr spectra of thse compounds have been interpreted, and the 13 Cn. mr spectra assigned with the aid of 2-D 13 C 1 H chemical-shift correlation spectroscopy. Tautomeric forms (furanoses, hydrate, and aldehyde) in solution in 2 H 2 O have been quantified with the aid of [1-13 C]- ...