Metal acetylides often serve as catalysts or reaction intermediates in synthetic processes. Among the metals used in combination with acetylene ligand, copper, silver, gold and iron predominate. In combination with these metals, many different ligands have been used for synthesis of these organometallic acetylide complexes. In this thesis, we have successfully synthesized copper and silver phenylacetylides. In addition, we have also prepared organometallic acetylides based on copper and gold with various selected ligands: e.g., 1,2-bis(diphenylphosphino)ethane (DPPE), phenanthroline and imidazole salt.