Layered hydroxide metal acetate Co2(OH)3(CH3COO)·H2O with an interlayer spacing of 1.282 nm has been synthesized by a novel method which is employed in ethanol-aqueous mixed solvents media.Experiment results show that the purity of the product by the modified method is higher compared with that by the previous methods.A complete characterization of the as-prepared samples was performed by means of X-ray powder diffraction,IR spectroscopy,scanning electron microscope,as well as magnetic measurement.The facile and effective approach for the preparation of this compound in this study is very interesting and important because it has wide application in the field of anionic exchange reaction for the synthesis of hybrid organic-inorganic compounds.