A 10 mL crimp vial equipped with a magnetic stirring bar was charged with the aliphatic heterocycle (0.2 mmol, 1 eq.), [Ir(dFCF3ppy)2dtbbpy]PF6] 3 (0.004 mmol, 0.02 eq., 4.4 mg), NiBr2 (dtbbpy) 3 (0.02 mmol, 0.1 eq., 9.7 mg and K2HPO4 (0.06 mmol, 0.3 eq., 10.4 mg). The vial was sealed, evacuated, and back filled with N2 for three times before adding anhydrous EtOAc (4.0 ml) to the reaction vial. Subsequently, the reaction mixture was then introduced to a nitrogen atmosphere via "freeze-pump-thaw" cycles (×3) with a syringe needle, keeping the vacuum approx. 7 mbar. After that the reaction mixture was irradiated with 5 W 450 (± 15) nm LEDs through the plane bottom side of the crimp vial (see Fig. for the reaction set up) and stirred intensely. The temperature was maintained at approx. 35 0 C by cooling with a builtin cooling fan. The reaction progress was monitored by GC or TLC analysis. After reaction completion, the reaction mixture was directly subjected for purification by silica gel flash column chromatography to isolate the desired product.