The intermolecular cobalt‐catalysed cyclotrimerisation of phenylacetylene as a benchmark alkyne with [1,2‐bis(4‐methoxyphenylthio)ethane]cobalt dibromide gave the symmetrical 1,3,5‐triphenylbenzene as the major product when dichloromethane was used as the solvent, whereas the unsymmetrical 1,2,4‐trisubstituted product was obtained in acetonitrile in quantitative yield. Optimisation of the aromatic and aliphatic disulfide ligands in different solvents is discussed.(© Wiley‐VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2008)
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