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Scaling up of continuous-flow, microwave-assisted, organic reactions by varying the size of Pd-functionalized catalytic monoliths

He, Ping; Haswell, Stephen J.; Fletcher, Paul D.I.; Kelly, Stephen M.; Mansfield, Andrew

Authors

Ping He

Stephen J. Haswell

Paul D.I. Fletcher

Andrew Mansfield



Abstract

A product-scalable, catalytically mediated flow system has been developed to perform Suzuki-Miyaura reactions under a microwave heating regime, in which the volumetric throughput of a Pd-supported silica monolith can be used to increase the quantity of the product without changing the optimal operating conditions. Two silica monoliths (both 3 cm long), with comparable pore diameters and surface areas, were fabricated with diameters of 3.2 and 6.4 mm to give volumetric capacities of 0.205 and 0.790 mL, respectively. The two monoliths were functionalized with a loading of 4.5 wt % Pd and then sealed in heat-shrinkable Teflon® tubing to form a monolithic flow reactor. The Pd-supported silica monolith flow reactor was then placed into the microwave cavity and connected to an HPLC pump and a backpressure regulator to minimize the formation of gas bubbles. The flow rate and microwave power were varied to optimize the reactant contact time and temperature, respectively. Under optimal reaction conditions the quantity of product could be increased from 31 mg per hour to 340 mg per hour simply by changing the volumetric capacity of the monolith. © 2011 He et al; licensee Beilstein-Institut.

Journal Article Type Article
Publication Date Aug 23, 2011
Journal BEILSTEIN JOURNAL OF ORGANIC CHEMISTRY
Print ISSN 1860-5397
Electronic ISSN 1860-5397
Publisher Beilstein-Institut
Peer Reviewed Peer Reviewed
Volume 7
Pages 1150-1157
APA6 Citation He, P., Haswell, S. J., Fletcher, P. D., Kelly, S. M., & Mansfield, A. (2011). Scaling up of continuous-flow, microwave-assisted, organic reactions by varying the size of Pd-functionalized catalytic monoliths. Beilstein Journal of Organic Chemistry, 7, 1150-1157. https://doi.org/10.3762/bjoc.7.133
DOI https://doi.org/10.3762/bjoc.7.133
Keywords Organic Chemistry
Publisher URL https://www.beilstein-journals.org/bjoc/articles/7/133

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