Synthesis of bis-arylsulfenyl-benzo-2,1,3-thiadiazoles was accomplished using a Pd-G3 XantPhos as a simple and inexpensive catalyst. Numerous benzene thiols reacted well with 4,7-dibromo-benzo-2,1,3-thiadiazole in DMF, using K2CO3 as the base, obtaining high product yields in a short reaction time. Furthermore, all the synthesized compounds showed remarkable fluorescent properties with emission wavelengths in the visible range. Due to their unique properties, they might be used as image probes in fluorescence microscopy. The study found that these compounds have a wide range of potential applications in the area of sensors, as well as other photophysical properties.