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Journal of Catalysis, Vol.306, 190-201, 2013
Experimental strategies for increasing the catalyst turnover number in a continuous Heck coupling reaction
This work presents a continuous Heck coupling reaction combined with organic solvent nanofiltration (OSN) separation of the catalyst in situ, using polymeric membranes at high temperature (80 C) and high concentration of base (>0.9 mol L-1). Two reactor configurations are investigated: a continuous single stirred tank reactor/membrane separator (m-CSTR) and a plug flow reactor (PFR) followed by m-CSTR (PFR-m-CSTR). The combined PFR-m-CSTR configuration was found to be the most promising, achieving conversions above 98% and high catalyst turnover numbers (TONs) of similar to 20,000. In addition, low contamination of the product stream (similar to 27 mg Pd per kg of product) makes this process configuration attractive for the pharmaceutical industry. (C) 2013 Elsevier Inc. All rights reserved.
Keywords:Continuous Heck coupling reaction;Pd retention in situ;Organic solvent nanofiltration (OSN);PEEK membrane;Low contamination of the product stream;High catalyst TON