A Design-of-experiment (DoE) strategy was used to optimise the process and gain a better understanding of which variables had the greatest statistical significance on the outcome. A definitive screen DOE was constructed using 17 initial experiments, augmented by a further 10 experiments to extend the range of each variable beyond the initial conditions. The yield of 2 was measured across an average of three samples per run. All statistical analysis and modelling were performed using JMP TM software. Modelling of the resultant data revealed that concentration of 1•PMDETA has the greatest statistical influence on yield, followed by gas pressure, then gas flow rate (Figure ).