Layered double hydroxide (LDH) comprising of Co2+ and La3+-ions with acetate counter anion was successfully synthe-sized by hydrogen peroxide catalyzed hydrolysis reaction and characterized extensively. The observed reflections in the powder X-ray diffraction pattern could be indexed inP3space group witha=0.316 nm andc=2.97 nm. Lattice fringes of distances corresponding to the peaks observed in X-ray diffraction pattern were observed in high resolution transmission electron microscopic images. UV-visible diffuse reflectance spectroscopy results confirmed the presence of Co(OH)6 along with the presence of charge-transfer band due to the interlayer carboxylate anion. Magnetization measurements at room temperature indicated high spin configuration of Co2+ -ion in the sample exhibiting paramagnetic behavior. The mixed metal oxide from calcination was used to reconstruct the parent layered structure. Intercalation experiments with other organic anions in Co-La LDH proved be successful.