MRT - Epoxidation

By: Matthias Junkers, Aldrich ChemFiles 2009, 9.4, 15.

Aldrich ChemFiles 2009, 9.4, 15.

Benefit from MRT & Flow Chemistry: 87% improvement in yield, better product quality, with safe & scale-independent handling of hazardous reagents and intermediates.

The batch synthesis of tetracyanoethylene oxide (311197) requires extended dosing times due to the exothermic nature of the reaction, however the product decomposes under reaction conditions and demands fast work-up. As already shown in previous examples, microreactor technology offers an ideal solution to this type of challenge (Scheme 8). Efficient heat transfer capabilities of microreactors allow very short contact times (τ < 3 min), where instant quenching of the product stream with water is easy to accomplish using a simple T-joint. Transfer of the synthesis from a batch to a flow process raised the product quality instantly from a yellow solid in only 23% yield, to a white powder in 43% yield without any optimization of the process. A considerable additional benefit is that the flow process can be scaled up without any further process development simply by prolonging the operation time. Scaling up the batch process would mean intensive additional work on the safety issues concerning the handling of accumulated large amounts of potentially hazardous oxygen compounds.

Scheme 8: Epoxidation (311197)(T8809)

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