Palladium continuous-flow microreactors

The aldol condensation/hydrogenation reaction was carried out in a continuous flow microreactor. The catalysts (0.5 g) were reduced in situ in a flow of H2 at atmospheric pressure at 723 K for 1 h for the palladium systems and 2 h for the nickel systems. The liquid reactant, acetone (Fisher Scientific HPLC grade >99.99%), was pumped via a Gilson HPLC 307 pump at 5 mL hr into the carrier gas stream of H2 (50 cm min ) (BOC high purity) where it entered a heated chamber and was volatilised. The carrier gas and reactant then entered the reactor containing the catalyst. The reactor was run at 6 bar pressure and at reaction temperatures between 373 and 673 K. Samples were collected in a cooled drop out tank and analyzed by a Thermoquest GC-MS fitted with a CP-Sil 5CB column... 

Metal-catalyzed cross-couplings are key transformations for carbon-carbon bond formation. The applicability of continuous-flow systems to this important reaction type has been shown by a Heck reaction carried out in a stainless steel microreactor system (Snyder et al. 2005). A solution of phenyliodide 5 and ethyl acrylate 6 was passed through a solid-phase cartridge reactor loaded with 10% palladium on charcoal (Scheme 2). The process was conducted with a residence time of 30 min at 130°C, giving the desired ethyl cinnamate 7 in 95% isolated yield. The batch process resulted in 100% conversion after 30 min at 140°C using a preconditioned catalyst. 

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