ortho-Heteroarylation of Azobenzenes by Rh-Catalyzed Cross-Dehydrogenative Coupling: An Approach to Conjugated Biaryls.

A direct cross-dehydrogenative coupling strategy for ortho-C-H activation and functionalization of azobenzenes with heteroarenes in the presence of a Rh catalyst was developed. Excellent regioselectivity was achieved by azo-coordinated Rh to realize oxidative C-H/C-H cross-coupling, providing a series of π-conjugated biaryls in good yields.