Ethynedithiol-based polyeneoligosulfides have been synthesized in 96% yield by the reaction of sodium acetylides (HCBCNa, NaCBCSNa) and elemental sulfur through the NaÀ ÀC sp bond in liquid ammonia with the following spontaneous polymerization of ethynedithiols (HSCBCSH) formed by the hydrolysis. The polyeneoligosulfides synthesized are brown powders (up to 77% sulfur content, mp 128-1848C), partially soluble in organic solvents.
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