Three new diols, 1, 2-di (2-naphthyl) ethane-1, 2-diol, 1-(l-naphthy1)-2-(2-naphthyl) ethane-l, 2-diol, and 1, 2-di (l-naphthyl) ethane-1, 2-diol, have been prepared in optically active form by catalytic asymmetric syn-dihydroxylation of the corresponding (E)-olefins. The complete stereochemical characterization was easily accomplished by transforming them into the corresponding isopropylidene ketals. These derivatives can be separated by HPLC on a ...