A simple and efficient method was developed for acylation of alcohols, using pillared clay catalyst such as {Fe-pillc, Cr-pillc, Cr-(Fe-pillc) and Fe-(Cr-pillc)} and a carboxylic acid as acylating agent. The pillared clay catalysts were calcined after incorporation of metal polycation ions with exchangeable cations and water. In the present study, the aliphatic alcohol (n-hexanol) and the aromatic alcohol (benzylalcohol) were acylated by using acetic acid and pillared clays. In these reactions it has been found that pillared clays have excellent catalytic activity. In direct acylation with acetic acid of alcohols (n-hexanol and benzylalcohol), pillared clays showed excellent catalytic activity. (C) 2004 Elsevier B.V. All rights reserved.