Ni hydrotalcites with different kinds of metals, ions exhibit considerable activity for organic transformations. Various ratios of Ni-Al hydrotalcites are prepared by using different compositions are characterized by XRD, IR and TPR analysis. Carbonate in the brucite sheets is active for selective oxidation reactions. Upon calcination the dehydroxylation of the hydrotalcite and concurrent decomposition of the carbonate ions produce mixed oxides which exhibits activity for variety of organic transformations.