This study contains a convenient synthesis and azo dye extraction efficiency of amino-functionalized calix[4]arene derivatives. Two calix[4]arene derivatives bearing alkyl amino groups on their upper and lower rim have been successfully synthesized and used as extractant for dye removal in liquid-liquid extraction system. The effect of electrolyte concentration, contact time, and pH on azo dye extraction was also investigated for all calixarene derivatives. From the results, it has been deduced that the amino-functionalized calix[4]arenes showed a better affinity than other parent calix[4]arenes towards the selected azo dyes.