Rhodium-catalyzed three-component C(sp 3 )/C(sp 2 )-H activation enabled by a two-fold directing group strategy.

Rh-catalyzed three-component C(sp 3 )/C(sp 2 )-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.