Disulfide sulflnates of the structure RSS(CH2)4SD2Na were synthesized by reaction of 1,2-dlthlane 1,1-dioxide (1), thiols, and sodium methoxlde In methanol. Disproportionation was minimized by precipitating and reprecipitating the products with ether as quickly as possible; where R = aryl, protection from light Is advisable. The groups R typify large llpophHIc ones ( -decyl, 1-adamantyl), small hydrophilic ones (2-carboxyethyl, 2,3-dlhydroxypropyl), disulfide sulflnates [(CH2)" SS(CH2)4SD2Na], and aryl groups substituted by electron-donating or electron-withdrawing groups. The products usually were quite hygroscopic and were Isolated as hydrates. They dlsproportlonated with varying ease In aqueous solution either to 1 or to the two symmetrical disulfides, RSSR and NaD2S(CH2)4SS(CH2)4SD2Na.