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A highly regioselective [Cp*Co(CO)I2]‐catalyzed addition of 1,3‐diketones to terminal alkynes at room temperature has been achieved using Cu(OTf)2 as a co‐catalyst. The reaction of 1,3‐diketones substituted at active methylene carbon with phenyl acetylenes having an electron‐withdrawing group or a bulky group results in the formation of the 2‐alkenylated 1,3‐dicarbonyl product, but phenyl acetylenes...
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