In the article it is mentioned about the synthesis of 2-hydroxy-5-(methylcycloalkyl)acetophenones from the acylation reaction of para-(methylacycloalkyl)phenols with acetic acid in the presence of ZnCl₂ as a catalyst. According to our studies, it was determined that the actual yield of 2-hydroxy-5-(methylcycloalkyl)acetophenones, which are synthesized from the acylation reaction of acetic acid with para-(1-methylcyclopentyl)-, para-(1(3)methylcyclohexyl)- and para-alkylphenols  which are obtained from  isoprene, piperylene and cyclodimers of divinyl in the presence ZnCl₂ as a catalyst, are 49.3–61.4%  in optimal conditions.