O,O '-(ortho-, meta-, or para-ditolyl) dithiophosphate ligands have been isolated as triethylammonium salts, (o-, m-or p-CH3C6H4O)2PS2HNEt3, by an auto-catalytic reaction of cresols with P2S5 in the presence of Et3N in a 4:1:2 molar ratio in toluene under anhydrous conditions. These triethylammonium salts could be converted into sodium/ammonium salts, (o-, m-, or p-CH3C6H4O)2PS2Na/NH4, by their direct reaction with sodium metal in equimolar ratio or passing dry ammonia gas in toluene. These salts were characterized by elemental analyses (C, H, N, and S) and mass, IR, and NMR (1H, 13C, and 31P) spectroscopic studies. [ABSTRACT FROM AUTHOR]