Titanium and zirconium 2-((p-tolylamino/p-tolylimino)methyl)phenolate (TAMP and TIMP) were prepared by reaction of Tiand Zr-alcoholates with 2-((ptolylamino)methyl)phenol (TAMPH) and 2-((p-tolylimino)methyl)phenol (TIMPH) in ethyl alcohol. To characterize these compounds, 1 H,
13C NMR, FTIR, mass spectroscopies, and elemental analysis were used. The TAMP and TIMP metal compounds can be formulated as (TAMP)3M2(OR)O2 and (TIMP)4M2O2, respectively. The catalytic activity of these compounds was checked in polymerization reactions with propylene oxide (PO) and ε-caprolactone (ε-CL) and Ti-TAMP was effective. Poly-propylene oxide (PPO) and poly-caprolactone (PCL) were identified by 1 H,
13C NMR and gel permeation chromatography (GPC).Keywords: Metal alkoxide, catalyst, Schiff base, ε-caprolactone, polymer.