The1H- and13C-NMR spectra of 6,7-dihalo-1,4-dihydro-4-oxo-1-(2,3,5-tri-0-benzoyl-pβ-D-ribofuranosyl)quinoline-3-carboxylic acids (3), (4), the ester (3a), 6-chloro-1-(2-deoxy-3,5-di-O-tolouyl-α- and β-D-erythropentofuranosyl)-7-fluoro-1,4-dihydro-4-oxo-quinoline-3-carboxylic acid (5), and its free a-nucleoside (5a) have been investigated. Resonance signals were assigned by homo- and heteronuclear two dimensional NMR methods (DQF-COSY, HMQC, and HMBC) for (3), (4), (5), and (5a). Ribosylation sites and anomeric configurations were identified from ROESY spectra.