The target of this work is to investigate structural and textural modifications of Li-Al hydrotalcite-like compounds by memory effect and their impact on the catalytic activity of these solids for the cyanoethylation reaction. The samples have been characterized by XRD, FT-IR. TG-DTG, surface area and porous structure. The catalytic test results showed that the reconstruction of the hydrotalcite leads to a decrease of the catalytic activity compared to the parent hydrotalcite. This fact may be related either to the smaller specific surface area of the reconstructed form or to the leaching of Li(+) during reconstruction. It has been also noticed that the calcination of Li-Al hydrotalcite leads to the formation of a alpha-LiAlO(2) stable phase. (C) 2010 Elsevier Ltd. All rights reserved.