Abstract Tetramethyl acetals of alkynedials were prepared by anodic oxidation of corresponding alkyne-1, ω-diols (C 4 and C 6) in trimethyl orthoformate on glassy carbone anode in 80% yield. 1, 1, 4, 4-Tetramethoxybut-2-yne (2a) can be prepared by this one-step procedure from but-2-yne-1, 4-diol (1a) instead of a multistep chemical procedure starting from 2, 5-dimethoxyfuran. Propargyl alcohol (3) can be similarly anodically oxidized in ...