Several layered double hydroxides (LDHs) containing metals of different nat
ure intercalated with benzoate anions have been synthesised in order to stu
dy the O-alkylation reaction of the interlayered species with alkyl halide
in dry media conditions. In all the cases, the expected ester was obtained
with good yield (> 60%). The presence of anionic benzoate in the structure
was prefered to obtain high selectivity and yield, in comparison with the u
se of sodium benzoate supported as a salt. The use of MW irradiation to pro
mote these reactions has permitted the reaction time to be reduced consider
ably. The influence of water present in the LDH on the ester formation has
also been investigated. Characterisation of the LDH support before and afte
r reaction is also presented, showing the influence of the nature of the ca
tions located in the octahedral sheets. The support can be regenerated, wit
h no effect on the reactivity.