TY - JOUR
T1 - Experimental strategies for increasing the catalyst turnover number in a continuous Heck coupling reaction
AU - Peeva, Ludmila
AU - Burgal, João da Silva
AU - Vartak, Shankul
AU - Livingston, Andrew G.
N1 - Funding Information:
This work was funded by the Novartis Pharma AG, Massachusetts Institute of Technology subaward Agreement No. 5710002924 ; The authors would like to acknowledge also the financial support from the U.K. Engineering and Physical Sciences Research Council (EPSRC) Grant No. EP/G070172/1 – ELSEP and the EC FP7 Ares(2011)1042335 – MEMTIDE .
Copyright:
Copyright 2013 Elsevier B.V., All rights reserved.
PY - 2013
Y1 - 2013
N2 - 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 ∼20,000. In addition, low contamination of the product stream (∼27 mg Pd per kg of product) makes this process configuration attractive for the pharmaceutical industry.
AB - 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 ∼20,000. In addition, low contamination of the product stream (∼27 mg Pd per kg of product) makes this process configuration attractive for the pharmaceutical industry.
KW - Continuous heck coupling reaction
KW - High catalyst TON
KW - Low contamination of the product stream
KW - Organic solvent nanofiltration (OSN)
KW - Pd retention in situ
KW - PEEK membrane
UR - http://www.scopus.com/inward/record.url?scp=84881160909&partnerID=8YFLogxK
U2 - 10.1016/j.jcat.2013.06.020
DO - 10.1016/j.jcat.2013.06.020
M3 - Article
AN - SCOPUS:84881160909
SN - 0021-9517
VL - 306
SP - 190
EP - 201
JO - Journal of Catalysis
JF - Journal of Catalysis
ER -
