In recent years, transition metal catalyzed C–H bond activation reactions are of considerable interest since such strategy can be used to reduce synthetic steps. Rhodium catalyst can undergo the oxidative coupling reaction with specific starting materials, and is one of the most effective methods to synthesize -conjugated molecules. Meta- and para-diaminobenzene, can be taken as starting materials of a acetylation reaction, which can produce substrates with diacetylatedamino groups on the benzene (which are needed for further oxidative coupling reactions.) The metal rhodium can catalyze an ortho C-H activation to make an oxidative coupling reaction of alkynes to produce the diacetylated product. This reaction can synthesize polysubstituted pyrrolo[3,2-f]indole and pyrrolo [2,3-f] indole derivatives.