A series of di-anionic cleavable surfactants were prepared by the condensation of aldehydes with 2,2- bis(hydroxymethyl)-1,3-propanediol, followed by reaction with 1,3-propanesultone in the presence of sodium hydride. Surfactant 5a had a differentH nuclear magnetic resonance spectrum in DO than products 5b−d. This was rationalized by its different conformation, which originates from the self-coiling of its alkyl chain. The critical micelle concentrations, Krafft points and hydrolysis properties of these surfactants were determined.