A new group of compounds, C(6)H(5)-N(O)=N-NH-C(6)H(4)-C(O)-O-C(6)H(4)-CH=N-C(6)H(4)-OR, (1), [R=n-alkyl group; 1 alpha (R=C(7)H(15)) to 1h (R=C(14)H(29))], has been designed and synthesized to develop triazene-1-oxide based liquid crystals. All the compounds have been characterized on the basis of their spectral data. Their thermal behavior has been examined and found to exhibit thermotropic liquid crystalline behavior over a wide range of temperature. All members of this family uniformly show nematic phase behavior on melting up to the clearing point during heating as well as on phase entering up to the solidification during cooling. An odd-even effect on transition temperatures has been observed during heating as well as cooling.