A new series of mesogenic unsymmetrical azines, N-(o-hydroxybenzylidene)-N 0 -(4-n-alkoxybenzoyloxybenzylidene)azines, HOC 6 H 4 CH=N-N=CHC 6 H 4 OCOC 6 H 4 O C m H 2m þ 1 (m ¼ 7, 8, 9, 10, 11, 12, 14, and 16) have been prepared. They have been characterized by elemental analyses, FT-IR, UV-visible, 1 H, and 13 C NMR (Nuclear Magnetic Resonance) spectra. The mesomorphic properties of these compounds were investigated by differential scanning calorimetry (DSC) and polarized optical microscopy (POM). The azines m ¼ 7, 10, and 14 exhibit features of enantiotropic nematic (N) mesophase whereas azines m ¼ 8, 11 exhibit features of a monotropic nematic phase. The azines m ¼ 9, 12, and 16 do not exhibit mesogenic nature.