The synthesis, diastereomeric separation, and characterization are described for a series of novel O-(2, 2, 2-trifluoroethyl)-3', 5'-dinucleoside phosphates, required for incorporation into antisense probes in the magnetic resonance imaging investigation of biodistribution. Preliminary assignment of the absolute configuration of the R p and S p diastereomers is made on the basis of 31 P NMR spectra.