C (sp3)–C (sp) bond formations are of immense interest in chemistry and material sciences. We report herein a convenient, radical-mediated and catalytic method for C (sp3)–C (sp) cross-coupling. Thus, with AgNO3 as the catalyst and K2S2O8 as the oxidant, various aliphatic carboxylic acids underwent decarboxylative alkynylation with commercially available ethynylbenziodoxolones in aqueous solution under mild conditions. This site- ...