The readily available (η⁴-COD)(triphenylphosphine)rhodium(I) acetate and trimethylsiloxide complexes have been established as useful precursors for generating the recently discovered rhodium(I) silyl complex, trans-(PPh₃)₂(η²-NBE)RhSiMe₂Ph, (COD = 1,5–cyclooctadiene, NBE = norbornene). A two-step sequence was used to first convert the (COD)(phosphine)rhodium acetate or siloxide complexes to the known (η³-cyclooctenyl)(bistriphenylphosphine)rhodium compound using one equiv. each of phenyldimethylsilane and triphenylphosphine. This intermediate, independently generated from the reaction of RhH(PPh₃)₃ and COD, was characterized by ¹H,¹³C,³¹P NMR spectroscopy. Subsequent treatment with additional hydrosilane and NBE released cyclooctene (COE) and generated the desired rhodium(I) silyl complex in a much slower reaction. Further details on the optimization of this reaction as a one-pot pot synthesis, reaction nuances, and characterization of salient rhodium complexes will be presented.