Four-dimensional nuclear magnetic resonance spectroscopy with high resolution of signals in the indirect dimensions is reported
as an implementation of the filter diagonalization method (FDM). Using an oligosaccharide derivatized with 13C-labeled acetyl isotags,
a four-dimensional constant-time pulse sequence was tailored for conjoint use with the FDM. Results demonstrate that high
resolution in all dimensions can be achieved using a relatively short experimental time period (19 h), even though the spectrum is
highly congested in the direct and all three indirect dimensions. The combined use of isotags, constant-time pulse sequences, and
FDM permits rapid isolation of sugar ring proton spin systems in multiple dimensions and enables all endocyclic J-couplings to
be simply measured, the key goal to assigning sugar stereochemistry and anomeric configuration. A general method for rapid, unambiguous
elucidation of spin systems in oligosaccharides has been a long-sought goal of carbohydrate NMR, and isotags combined
with the FDM now enable this to be easily performed. Additional general advantages of the FDM program for generating highresolution
2D slices in any dimension from a 4D spectrum are emphasized.