Gem-dihydroperoxides which have been much important in recent years due to their relevance to peroxidic anti-malarial drugs are stable derivatives of aldehydes and ketones [1]. These compounds are useful and vital key intermediates in synthesis of many classes of peroxides, such as tetraoxanes [1] and other tetraoxacycloalkanes, [2] macrocyclic endoperoxides, [3] and acyclic analogues with a variety of functional groups [4]. In addition, recently gem-dihydroperoxides have been used as suitable and powerful oxidant in some organic reactions [4]. In this research, we have used antimony (III) chloride (SbCl ) as a new, efficient and commercially available simple catalyst for conversion of different aldehyde and ketones to corresponding gem-dihydroperoxides in high yields and purity (scheme 1). Time of reactions are short to moderate. Finally, it seems that conditions of reactions are mild and methods of purifications are simple.3