The defluorosilylation of HCF3 with 1•PMDETA was conducted in flow using a Vapourtec easy-scholar reactor system (Figure ). A reactor coil of length = 495 cm, volume = 3.9 ml was used, leading to residence times of between 30 s -6 min depending on flow rates used. All reactions were conducted at 25 °C. Flow rates were regulated to initially produce a segmented flow regime directly after the T-junction, however, as the reaction proceeded HCF3 was consumed resulting in dissipation of the segmented flow. Samples for analysis were collected following dispensing of 1 to 2 reactor volumes under flow. Precipitation of a solid, presumed to be LiF, was observed during reactions but did not cause fouling of the reactor tubing. Formation of 2 was quantified by both F NMR spectroscopy and GC-FID analysis.