Investigation began with the substrate 3a. Initially commonly employed hydroperoxidation conditions developed by Mukaiyama were used followed by treatment under a variety of reducing conditions (Fig. , Entry 1) . However, survey of a wide variety of conditions did not lead to the desired reduced compounds derived from β-scission. Ferrous sulfate, copper(II) tetrafluoroborate, and copper (II) sulfate, and others were investigated, with multiple unidentified products formed without the observation of the desired product. Various solvents (MeOH, DCE, DMF, i-PrOH, DCM, etc.) and combinations thereof were also examined. When silylhydroperoxidation was attempted followed by treatment under reducing conditions, the product could be observed.