The protocol, 3-methyldec-1-yn-3-ol (1a) was chosen to perform the dimerization process. The optimal conditions for synthesis of 8,13-dimethylicosa-9,11-diyne-8,13 (2a) with high efficiency when using copper-catalyzed, N,N,N′N′-tetramethylethylenediamine as a ligand and CCl4 and methanol solvents in atmospheric pressure were determined. The structure of the obtained compound was proved by IR, 1H-NMR and 13C-NMR spectroscopy.