reflected into an increase in yield to 40%. It is important to note that an excess of gas reagent should not pose any problem, as it can be easily recovered and recycled after the reaction by simply reducing pressure to atmospheric pressure, thus ensuring phase separation between the gas and liquid phases. Increasing the TBADT loading to 2.5 mol% (entry 5) led to a further rise in the chemical efficiency. At this stage of the optimization, several ligands for the Ni catalyst were screened, with 4,4′-di-tert-butyl-2,2′-dipyridyl confirming its superior activity (See Supplementary Information, Section 4). An assessment of several reaction additives and solvent mixtures highlighted the positive impact of LiBr and tBuOH (entries 6 and 7). Although extending the residence time to 30 minutes (entry 8) and implementing a recirculation system to increase reaction times even further to 50 minutes (entry 9) resulted in only a minor increase in chemical efficiency, the introduction of a fresh solution of TBADT before the recirculation step (entry 10, See Supplementary Information, Section 4.6) furnished the desired compound 2 in a 60% yield.