3D printed materials can be readily modified to create bespoke structures that incorporate a range of catalysts at the point of printing. In this present study we report on the...

3D printed materials can be readily modified to create bespoke structures that incorporate a range of catalysts at the point of printing. In this present study we report on the design and 3D printing of tetrakis (triphenylphosphine) palladium (0) impregnated 3D printed stirrer devices that were used to catalyze a Suzuki-Miyaura reaction between biaryl compounds in a batch-based approach. It was shown that the devices themselves are reusable, easy to use, air-stable, give access to an array of biaryl compounds in excellent yields and lead to low levels of palladium loss into the reaction. Simple modification of the device’s design by size reduction, meant that they could also be used to reduce the time of the Suzuki-Miyaura reaction by microwave enhanced heating. At the end of the reaction, devices can simply be removed from the flask, washed and reused, analogous to stirrer bead workflows. This makes the overall process of setting up multiple reactions simpler by obviating the need to weigh out catalysts for reactions and the device, once used, can be simply removed from the reaction media at the end of the reaction.

The structures of two novel pyridinium catecholates are reported by reaction of pyridine with tetrachloro-o-benzoquinone and tetrabromocatechol; with tetrachlorocatechol pyridine acts as a base with the structure of the pyridinium-catecholate salt reported.

3D printed materials can be readily modified to create bespoke structures that incorporate a range of catalysts at the point of printing. In this present study we report on the design and 3D printing of tetrakis (triphenylphosphine) palladium (0) impregnated 3D printed stirrer devices that were used to catalyze a Suzuki-Miyaura reaction between biaryl compounds in a batch-based approach. It was shown that the devices themselves are reusable, easy to use, air-stable, give access to an array of biaryl compounds in excellent yields and lead to low levels of palladium loss into the reaction. Simple modification of the device’s design by size reduction, meant that they could also be used to reduce the time of the Suzuki-Miyaura reaction by microwave enhanced heating. At the end of the reaction, devices can simply be removed from the flask, washed and reused, analogous to stirrer bead workflows. This makes the overall process of setting up multiple reactions simpler by obviating the need to weigh out catalysts for reactions and the device, once used, can be simply removed from the reaction media at the end of the reaction.

We describe the development of Lewis Acid catalyst-impregnated 3D printed stirrer devices and demonstrate their ability to facilitate the rapid screening of reaction conditions to synthesize heterocycles. The SLA 3D printed stirrer devices were designed to fit round-bottomed flasks and Radleys carousel-tubes using our recently reported solvent resistant resin and using CFD modelling studies and experimental data, we demonstrated that the device design leads to rapid mixing and rapid throughput over the device surface. Using a range of Lewis Acid 3D printed stirrers, the reaction between a diamine and an aldehyde was optimized for catalyst and solvent and we demonstrated that use of the 3D printed catalyst embedded devices led to higher yields and reduced reaction times. A library of benzimidazole and benzothiazole compounds were synthesized and use of devices led to efficient formation of the product as well as low levels of catalyst in the resultant crude mixture. The use of these devices makes the process of setting up multiple reactions simpler by avoiding weighing out of catalysts and the devices, once used, can be simply removed from the reaction, making the process of compound library synthesis more facile.