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He P, Haswell SJ, Fletcher PD, et al. Scaling up of continuous-flow, microwave-assisted, organic reactions by varying the size of Pd-functionalized catalytic monoliths. Beilstein J Org Chem. 2011;7:1150-7doi: 10.3762/bjoc.7.133.
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, 71150-7. https://doi.org/10.3762/bjoc.7.133
He, Ping, et al. "Scaling up of continuous-flow, microwave-assisted, organic reactions by varying the size of Pd-functionalized catalytic monoliths." Beilstein journal of organic chemistry vol. 7 (2011): 1150-7. doi: https://doi.org/10.3762/bjoc.7.133
He P, Haswell SJ, Fletcher PD, Kelly SM, Mansfield A. Scaling up of continuous-flow, microwave-assisted, organic reactions by varying the size of Pd-functionalized catalytic monoliths. Beilstein J Org Chem. 2011;7:1150-7. doi: 10.3762/bjoc.7.133. Epub 2011 Aug 23. PMID: 21915220; PMCID: PMC3170192.
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Beilstein J Org Chem. 2011;7:1150-7. doi: 10.3762/bjoc.7.133. Epub 2011 Aug 23.

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

Beilstein journal of organic chemistry

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

Affiliations

  1. Department of Chemistry, University of Hull, Hull HU6 7RX, UK.

PMID: 21915220 PMCID: PMC3170192 DOI: 10.3762/bjoc.7.133

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.

Keywords: Suzuki–Miyaura reaction; continuous flow; microwave heating; monolith; scaling-up

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