In the research described below, we have developed a convenient and effective method of synthesis of organic peroxyesters to achieve 60-98% yields under extreme mild conditions. The study has been conducted on a model system using a reaction of acylation of 1-methyl-1-phenylethyl hydroperoxide (CHP) by means of butyryl chloride in the presence of solid Na2CO3 and being performed under conditions of phase transfer catalysis (PTC). The effect of the following parameters on the reaction was tested: temperature, Na2CO3 amount, catalyst structure and solvent polarity.