C( sp ³ )–H Activation/Cleavage of Alcohols and C–C Coupling with Nonactivated Alkenes through Rhodium Catalysis Triggered by O ₂

)-H activation of alcohols, enabling C-C coupling with nonactivated alkyl-substituted alkenes. The transformation proceeds with high chemo- and regioselectivity and achieves 100% atom economy. A variety of secondary alcohols are synthesized in yields of 11% to 92% under simple and mild conditions. Mechanistic studies indicate that the reaction proceeds via a C-H activation and radical addition pathway.