Unsymmetric diynes possessing a terminal alkyne moiety reacted with organoboronic acids both chemo-and stereoselectively to afford arylated or alkenylated exocyclic dienes by catalysis from the [Rh(cod)OCH 3 ] 2 complex. The use of a polar protic solvent, e.g. CH 3 OH is required for the success of the process under mild conditions.
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