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A gold-catalyzed tandem alkyne oxidation/C-H functionalization has been realized in aqueous media.1 Importantly,it was revealed for the first time that water could dramatically inhibit the undesired overoxidation,which might serve as a general solution to the overoxidation in oxidative gold catalysis.In addition,a zinc(Ⅱ)-catalyzed tandem alkyne oxidation/C-H functionalization has also been achieved,where the relevant over-oxidation can be completely suppressed.