The synthesis and measurement of physical properties using DSC, X-ray and optical methods are described for the 3,5-bis-(p-n-alkoxyphenyl)-pyrazole and 3,5-bis-(p-n-alkoxyphenyl)-isoxazole series with the carbon number of then-alkylgroup from three to eight. The pyrazole series with longern-alkylgroups (n= 6, 7, and 8) show the smectic A (SmA) as well as smectic C (SmC) phases. The corresponding isoxazole compounds show nematic (N) and alsoSmAphases. The compounds with shortern-alkylgroups (n= 3, 4 and 5) show either nematic orSmAphases for both series respectively.