The synthesis of novel dithiophosphate derivatives has been achieved. Two O,O-alkanediyl S-(N-phthalimidomethyl) dithiophosphates and two Zinc bis(O,O-alkanediyl) dithiophosphates are synthesized by an easy and facile chemical synthetic route. Zinc bis[O,O-(2-methylpentane-2,4-diyl) dithiophosphate] L-1, Zinc bis[O,O-(2-ethylhexane-1,3-diyl) dithiophosphate] L-2, O,O-(2-methylpentane-2,4-diyl) S-(N-phthalimidomethyl) dithiophosphate L-3 and O,O-(2-ethylhexane-1,3-diyl) S-(N-phthalimidomethyl) dithiophosphate L-4 are synthesized from the respective ammonium salts. Compounds L-1, L-2, L-3, and L-4 are characterized by (CHN) elemental analysis, ESI mass, FT-IR, H-1, C-13, and P-31 NMR techniques. The crystal structure of ammonium O,O-(2-methylpentane-2,4-diyl) dithiophosphate is discussed. L-1, L-2, L-3, and L-4 were evaluated for antimicrobial activity. It was found that the phthalimide derivatives L-3 and L-4 showed much better antifungal potential against some species of fungus. The Zinc dithiophosphates L-1 and L-2 showed good antibacterial activity against Bacillus cereus and Escherichia coli.