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<p>The synthesis of conjugated triynes by
molybdenum-catalyzed alkyne metathesis is reported.
Strategic to the success of this approach is the utilization
of sterically-hindered diynes that allowed for the site-
selective alkyne metathesis to produce the desired con-
jugated triyne products. The steric hindrance of alkyne
moiety was found to be crucial in preventing the for-
mation of diyne byproducts. This novel synthetic strategy
was amenable to self- and cross-metathesis providing
straightforward access to the corresponding symmetrical and dissymmetrical triynes with high selectivity.
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