Abstract
The Pd-catalyzed aminocarbonylation of aromatic bromides was investigated in both a silicon microreactor and a packed-bed tubular reactor. An automated transient temperature ramp method with in-line IR analysis led to significantly more rapid determination of reaction kinetics than traditional steady-state screening for offline GC analysis.
Highlights
The carbonyl group is one of the key building blocks of nature, where it is essential for the construction of proteins, many polymers, and numerous drugs
A residence time of 3 minutes was realized with a CO mass flow rate of 0.96 sccm at a pressure of 8.3 bar, corresponding to a CO gas phase concentration of 0.37 M, and a liquid phase p-bromobenzonitrile concentration of 0.1 M
The applicability of the system was proven for the successful carbonylation of aryl bromides
Summary
The carbonyl group is one of the key building blocks of nature, where it is essential for the construction of proteins, many polymers, and numerous drugs. While numerous single-phase automated screening studies are known, two-phase gas–liquid systems are more complex, and, as a result, there are significantly fewer examples of automated screenings across multiple reaction variables.[30,31] In our initial study, the 230 μL silicon nitride spiral reactor and the activated aryl bromide, p-bromobenzonitrile (4), were used (Scheme 2).
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