A series of novel azomethinediols, benzene 1,4-di(4-iminohydroxyphenoxy-n-alkanol)s was prepared from 4-[4-(4-hydroxybenzylideneamino)phenyliminomethyl] phenol with 2-chloroethanol, 3-bromopropanol, 6-bromohexanol, respectively. A series of poly(azomethine-urethane)s was prepared by condensation of benzene 1,4-di(4-iminohydroxyphenoxy-n-alkanol) with hexamethylene-diisocyanate (HMDI), isophorone-diisocyanate (IPDI), 4,4'-methylene-di(phenyl-diisocyanate) (MDI) and 2,4-toluylene-diisocyanate (2,4 TDI), respectively. Thermotropic liquid crystalline properties of these synthesized poly(azomethine-urethane)s were examined by differential scanning calorimetry (DSC), optical photomicroscopic observation, X-ray diffraction and thermogravimetric analysis (TGA). All of the polymers, except polymers P2, P3 and P7, exhibit thermotropic liquid crystalline properties.