In this work, we report on the synthesis, characterization, and antifungal activities of new boron derivatives of O-alkyl or O-aryl trithiophosphate of the type ROP(S)S 2 [BS 2 P(S)OR] 2 ·2NMe 3 (R = Me, Et, Pr i , Bu i , Ph, CH 2 Ph). They were synthesized by the reaction of trimethylaminoborane with O-alkyl or O-aryl trithiophosphate in 2:3 molar ratio in dried and distilled benzene. The newly synthesized derivatives are light yellow viscous liquids, monomer, and soluble in common organic solvents. These compounds have been characterized by elemental analysis, molecular weight determinations, and spectroscopic (IR, 1 H, 11 B, and 31 P NMR) studies which are consistent with four-coordinated boron and bidentate behavior of the trithiophosphate moiety. It is observed that when these derivatives are applied in the form of dilute solution in ethanol of various concentrations, they show their effectiveness against powdery mildew disease at a fixed interval of days.