A convenient and high-yield synthesis of alkylphosphine and mixed alkylarylphosphine derivatives of Vaska’s complex, trans-Ir(PPh3)2(CO)Cl, is reported. The procedure involves the addition of phosphines to cis-Ir(CO)2Cl[NH2(p-C6H4Me)], resulting in the elimination of a CO and eventually the amine ligand upon heating. The product yields are in the range 70-80%. In addition to giving a much better yield, this procedure eliminates the need for using different starting materials for different phosphines, as required by the previously reported methods.