Alkanedisulfamic acid functionalized silica-coated magnetic nanoparticles (ADSA-MNPs) were used as effective, low-cost and reusable solid heterogeneous nanomagnetic catalysts for conversion of aldehydes and ketones to corresponding gemdihydroperoxides and 1,2,4,5-tetraoxanes using aqueous hydrogen peroxide (30% w/w in H2O) at room temperature. These compounds are important key intermediates in preparation of anti-malaria drugs. The reactions proceeded in high rates and excellent yields. Since the catalyst was separated facilely from the reaction mixture by an external magnet and was reused six times without considerable loss of catalytic activity, this methodology is environmentally friendly. It is notable that it is the first report on using a nanocatalyst in the synthesis of gem-dihydroperoxides and 1,2,4,5-tetraoxanes from aldehydes and ketones up to now.