[RhCp*(OAc)(2)(H2O)] [Cp* = pentamethylcyclopentadienyl] catalyzed the C-H bond amidation of ferrocenes possessing directing groups with isocyanates in the presence of 2 equiv/Rh of HBF4 center dot OEt2. A variety of disubstituted ferrocenes were prepared in high yields, or excellent diastereoselectivities.