Metal-organic frameworks (MOF) are studied extensively in applications like catalysts, gas storage, and sensors due to their various functional groups and structures. Two-dimensional (2D) MOFs such as triphenylene-based materials show excellent charge transport properties, but thin-film fabrication and organic ligand synthesis are difficult. In this work, we synthesize thiol-based organic ligand, benzenehexathiol (BHT), by a simple one-pot reaction. This facile method is safer and faster than conventional synthesis procedure that requires using liquid ammonia as solvent. Two novel 2D MOF materials, Ag3BHT2 and Au3BHT2, are fabricated by coordinating BHT with either silver (Ag) or gold (Au) ions through liquid-liquid interfacial reaction. The Ag3BHT2 thin film reaches a high electrical conductivity of 363 S cm-1, which has potential applications in electronic devices and sensors.