Tetrakis(p‐tolyl)oxalamidinato‐bis[acetylacetonatopalladium(II)] ([Pd2(acac)2(oxam)]) reacted with Li–C≡C–C6H5 in THF with formation of [Pd(C≡C–C6H5)4Li2(thf)4] (1a). Reaction of [Pd2(acac)2(oxam)] with a mixture of 6 equiv. Li–C≡C–C6H5 and 2 equiv. LiCH3 resulted in the formation of [Pd(CH3)(C≡C–C6H5)3Li2(thf)4] (2), and the dimeric complex [Pd2(CH3)4(C≡C–C6H5)4Li4(thf)6] (3) was isolated upon reaction of [Pd2(acac)2(oxam)] with a mixture of 4 equiv. Li–C≡C–C6H5 and 4 equiv. LiCH3. 1–3 are extremely reactive compounds, which were isolated as white needles in good yields (60–90%). They were fully characterized by IR, 1H‐, 13C‐, 7Li‐NMR spectroscopy, and by X‐ray crystallography of single crystals. In these compounds Li ions are bonded to the two carbon atoms of the alkinyl ligand. 1a reacted with Pd(PPh3)4 in the presence of oxygen to form the already known complexes trans‐[Pd(C≡C–C6H5)2(PPh3)2] and [Pd(η2‐O2)(PPh3)2]. In addition, 1a is an active catalyst for the Heck coupling reaction, but less active in the catalytic Sonogashira reaction.
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