We
report the development of a small footprint continuous electrochemical
Taylor vortex reactor capable of processing kilogram quantities of
material per day. This report builds upon our previous development
of a scalable photochemical Taylor vortex reactor (Org. Process
Res. Dev.
2017, 21, 1042; 2020, 24, 201–206). It describes a
static and rotating electrode system that allows for enhanced mixing
within the annular gap between the electrodes. We demonstrate that
the size of the annular gap and the rotation speed of the electrode
are important for both conversion of the substrate and selectivity
of the product exemplified using the methoxylation of N-formylpyrrolidine. The employment of a cooling jacket was necessary
for scaling the reaction in order to manage the heat generated by
electrodes at higher currents (up to 30 A, >270 mA cm–2) allowing multimole productivity per day of methoxylation product
to be achieved. The electrochemical oxidation of thioanisole was also
studied, and it was demonstrated that the reactor has the performance
to produce up to 400 g day–1 of either of the corresponding
sulfoxide or sulfone while maintaining a very high reaction selectivity
(>97%) to the desired product. This development completes a suite
of vortex reactor designs that can be used for photo-, thermal-, or
electrochemistry, all of which decouple residence time from mixing.
This opens up the possibility of performing continuous multistep reactions
at scale with flexibility in optimizing processes.
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