In the presence of a palladium(0) complex catalyst, methoxymethyldisilanes, (MeO)n Me3-nSiSiMe3-m (OMe)m (m, n 1, 2), added to 1-hexyne, trimethylsilyl-acetylene and acetylene to give double silylation products, 1,2-bis(methoxy-methylsilyl)olefins, in varying yields.