Cyclometalated Pt(II) β-diketonates are widely used as efficient luminescent materials but are typically prepared at high temperatures in low yields using excess reagents. A one-pot synthesis of these complexes is described employing stoichiometric reagents and short reaction times at ambient temperature, giving yields of up to 94%. The method is applicable to a broad range of substrates including N^C, P^C, and C^C chelate Pt(II) complexes and different β-diketonate ligands.