Herein, two new azo reagents, 2-[(1-banzimidazol)azo]-2-hydroxy-5-banzal (BIApB) and 6-[(1-banzethiazol) azo thymol] (BTAT), were synthesized and identified using FTIR, UV-Vis, mass spectrometry, and ¹H-NMR. Also, this research presents a comparative analysis of novel azo-chelating reagents for the cloud point extraction (CPE) of gold complexes. The study evaluates how the structural differences between the benzimidazole and benzothiazole moieties influence both extraction efficiency (E%) and th