AbstractSynthetic methodologies for the preparation of nitroxyl labeled derivatives of D -(+)-glucose, α -D -(+)-m ethylglycoside, 2-amino-2-deoxy-D -(+)-glucose, and D -(+)-glucuronic acid are presented. The spin labels in these compounds are attached variably at the 1, 2, 3, and 6 positions of the glucose framework. These new compounds, being water soluble and producing marked enhancement of spin-lattice (T ,) and spin-spin (T2) proton relaxation in deionized water and human plasma have potential utility as contrast altering pharmaceuticals for magnetic resonance imaging and as spin probes in biomolecular research. These spin labeled carbohydrates may demonstrate in vivo biodistribution characteristics reflecting tissue-specific differences in glucose metabolism .