The synthesis and mesomorphic properties of a novel azoester homologous series consisting of 12 members is reported. The methyl to butyl derivatives of the series are non-mesogenic, and the others are enantiotropically smectogenic and/or nematogenic. The nematic mesophase shows a threaded or Schlieren texture and smectic mesophase shows a focal conic fan-shaped texture of the SmA or the SmC. The smectic and nematic thermal stabilities are 137.4 degrees and 166.6 degrees respectively. Analytical data support the molecular structures. The transition temperatures of the homologues are determined using optical polarizing microscopy. An odd-even effect is observed for the nematic-isotropic transition curve and the series is equally smectogenic and nematogenic over a wide temperature range, and the melting points are in the middle order. The mesogenic properties of the present series are compared with a structurally similar homologous series.