Gem-dihydroperoxides that are stable peroxidic derivatives of ketones and aldehydes, have been remarkable compounds because of their relevance toperoxidic anti-malarial drugs [1]. Also, these compounds are important intermediates in the synthesis of a number of classes of peroxides including tetraoxanes, silateraoxans, spirobisperoxyketals, bisperoxyketals, 1,2,4,5-tetraoxa cycloalkanes[2]. Recently, for synthesis of these germinal peroxides ketones and aldehydes have been reacted with H2O in presence of Lewis acids in organic solvents. Several Lewis acids such as I22, CAN reagent, CSA, NaHSO4 and PMA have been used for this conversion[3].Gem-dihydroperoxides have also been employed as reagents for oxidation reactions such epoxidation of a, ß-unsaturated ketones, enantioselective oxidation of 2-substituted 1, 4-naphtoquinones, oxidation of sulfide and as suitable oxidants in other organic reactions [4]. As importance of these compounds, we have been improved them synthesis by using some green, inexpensive, commercially available and effective catalyst. [4]Also, we have been reported first time synthesis of trans-3,5-dihydroperoxy-3,5-dimethyl-1,2-dioxalane as an efficient, powerful and solid cyclic gem-dihydroperoxide and we used it in many oxidative organic reaction (scheme 2).