A synthetic procedure for optically active and racemic α-nitronyl nitroxides (α-NNs) having a stereogenic center at the 4-position of the imidazolyl ring is described. This procedure consists of (1) the synthesis of a dissymmetric vic-dinitro compound by Kornblum reaction,(2) the enantiomeric resolution of the racemate by a diastereomer method for obtaining the optically active sample,(3) the quick reduction of the optically active or racemic vic-dinitro ...