MgAl and MgMAl oxides(M = Co,Ni and Cu) with a Mg:M:Al molar ratio = 4:1:1 were synthesized from the calcination of their corresponding layered double hydroxide(LDHs) precursors.Their catalytic activities were examined for the oxidation of ethylbenzene using tert-butylhydroperoxide(TBHP) as an oxidant.The oxidized product was mainly acetophenone.The catalytic activities were in the order of MgCuAl>MgNiAl～NiAl～MgCoAl～CoAl>CuAl>MgAl oxides.Reusability studies show that the catalysts are stable under the reaction conditions. MgAl and MgMA oxides (M = Co, Ni and Cu) with a Mg: M: Al molar ratio = 4: 1: 1 were synthesized from the calcination of their corresponding layered double hydroxide (LDHs) precursors. Their catalytic activities were examined for the oxidation of ethylbenzene using tert-butylhydroperoxide (TBHP) as an oxidant. The oxidized product was mainly acetophenone. the catalytic activities were in the order of MgCuAl> MgNiAl ~ NiAl ~ MgCoAl ~ CoAl> CuAl> MgAl oxides. catalysts are stable under the reaction conditions.