Reaction of isopropyl[(2-pyridyl)alkyl]amines such as N-isopropyl-N-2-methylpyridine or N-isopropyl-N-2-ethylpyridine with aqueous solutions of NaAuCl 4 led to the formation of [LAuCl 2 ][AuCl 4 ] in low yields, where L=pyridyl amine bound to gold in a bidentate fashion. Reaction of 2-(3,5-diphenyl-1H-pyrrol-2-yl)pyridine with aqueous NaAuCl 4 , however, proceeded with formal loss of HCl and direct formation of the gold(III) amido complex L′AuCl 2 , where L′=deprotonated pyrrolyl ligand. Optimization of the reaction conditions to make the new amido complex identified MeCN:H 2 O (1:2) as the best choice of solvent, affording product in 92% yield. This dichloro amido complex is a convenient precursor to L′AuMe 2 , which was found to be air-stable and thermally robust.