A novel catalytic system of AgOTs-CuCl2-TMEDA is described for the homocoupling of aliphatic acetylenes on solid support. It is the first observation that Ag-l's activating triple bond could facilitate Cu-II-mediated oxidative acetylenic homocoupling. This study provides an efficient way to synthesize a diversified symmetrical bis-benzo[b]furan-linked 1,3-diyne library on solid support.
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