A process is disclosed for the preparation of a dialkyl peroxide comprising reacting one or more members selected from the group consisting of an alkylating alcohol of the formula ROH, and an olefin of the formula (R2)(R2a)CC(R3)(R3a), wherein R is C1-C10 allyl, and R2, R2a, R3, and R3a are independently selected from hydrogen and C1-C10 alkyl; with a hydroperoxide of the formula R1OOH, wherein R1 is C1-C10 allyl; in the presence of an effective amount of a substantially solid, insoluble, heterogenous acidic catalyst; followed by separation of the reaction mixture from said catalyst; wherein said catalyst has readily available acidity for organic reactions and exists in the solid phase in the processes of the invention, while the reactants in those processes, by contrast, exist in the liquid and/or gaseous phase, whence the catalyst is referred to as heterogeneous.

 
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