Abstract: | A triple catalytic system designed for asymmetric dihydroxylation of olefins, composed of NMM and two divergent heterogeneous catalysts, titanium silicalite and silica gel‐supported 1,4‐bis(9‐O‐dihydroquinidinyl)phthalazine SGS‐(DHQD)2PHAL)]‐OsO4 complex relays the transport of two electrons from olefin to H2O2 used as a terminal oxidant to provide chiral diols with good yields and high enantiomeric excesses in a single pot. |