Bisphosphodiester surfactant is a name assigned to a family of synthetic amphiphiles possessing a hydrocarbon chain attached to another hydrocarbon chain via different methylene chains as a spacer derived from α-ω-alkyl dibromide (1,4-DBB, 1,6-DBH and 1,8-DBO). In the present study, a series of bisphosphodiester surfactants having C 14 hydrophobic tail and different methylene chains as a spacer derived from α-ω-alkyl dibromide have been synthesized at 35°C. The effect of reaction variables like temperature, duration and molar ratios of mono tetradecyl phosphate, tetramethyl ammonium hydroxide and spacer on the yield of bisphosphodiester surfactants has also been reported. Modern instrumental techniques viz. FT-IR, 1 HNMR, and 13 CNMR were utilized to characterize the functional groups presence in synthesized bisphosphodiester surfactants. Elemental analysis of synthesized bisphosphodiester surfactants was also carried out. Surface active properties viz. surface tension, interfacial tension, critical micelle concentration and aqueous properties viz. foaming stability, wetting ability, emulsifying ability and dispersing power of synthesized gemini surfactants were also determined. Among all synthesized bisphosphodiester surfactants IIIb had maximum anionic content of 78.9%; and showed highest foaming ability (70 ml), superior dispersing ability (45.7%), whereas IIIc showed low CMC values (0.00026 mmol/l); minimum surface tension and interfacial tension (37.3 mN/m and 31.6 mN/m) respectively.