Process for preparing 2,2'-diacetoxy-dibenzoylperoxide by: reacting 2-acetyl-salicyloyl chloride with aqueous hydrogen peroxide in a reaction mixture medium of tetrahydrofuran and dichloromethane in the presence of an organic base; separating a dichloromethane extract; diluting the dichloromethane extract with methanol and crystallizing the anhydrous product therefrom.