Rhodium-catalyzed three-component C(sp3)/C(sp2)–H activation enabled by a two-fold directing group strategy.

Rh-catalyzed three-component C(sp3)/C(sp2)–H activation has been achieved through a two-directing group strategy. This protocol provides a convenient and efficient pathway for the construction of diverse 8-alkyl quinoline derivatives in one-pot. Furthermore, mechanistic studies revealed that the first C–H amidation was significantly faster than the sequential C–H alkylation. [ABSTRACT FROM AUTHOR]