Abstract: Nickel acetylacetonate was synthesized with acetylacetone and the nickelous chloride, and two -Ketone imine ligand was synthesized with acetylacetone and aromatic amines. In this paper, the product was characterized by IR and UV spectrum, and their thermal properties was study by DSC. Meanwhile the process of Schiff base synthesis method to improve yield is also discussed in the paper. Finally the possible mechanism of the active site of catalytic nickel acetylacetone/ Triphenyl phosphine was speculated through the UV spectra .