Translating solid state organic synthesis from a mixer mill to a continuous twin screw extruder

Abstract

A study on the translation of a solid-state synthetic reaction from a mechanochemical mixer-mill to a continuous twin-screw extruder is discussed herein. The study highlights some considerations to be made and parameters to be tested in the context of a model fluorination reaction, which is the first organic fluorination to be attempted using extrusion. Upon optimization, which features the first use of grinding auxiliary solids to enable effective synthetic extrusion, the difluorination reaction was successfully translated to the extruder, leading to a 100-fold improvement in Space Time Yield (STY); 29 kg m⁻³ day⁻¹ in a mixer mill to 3395 kg m⁻³ day⁻¹ in a twin screw extruder.