Protocol for Automated Kinetic Investigation/Optimization of the RAFT Polymerization of Various Monomers

• Published in: QSAR & combinatorial science Vol. 27; no. 8; pp. 977 - 983
• Main Authors: Becer, Caglar Remzi, Groth, Andrew M., Hoogenboom, Richard, Paulus, Renzo M., Schubert, Ulrich S.
• Format: Journal Article
• Language: English
• Published: Weinheim WILEY-VCH Verlag 01-08-2008; WILEY‐VCH Verlag
• Subjects: Automated parallel synthesis; Controlled/living polymerization; High-throughput experimentation; Optimization protocol; Polymerization kinetics
• ISSN: 1611-020X; 1611-0218
• DOI: 10.1002/qsar.200720159

A standard protocol for the parallel optimization of Reversible Addition–Fragmentation Chain Transfer (RAFT) polymerization conditions using an automated synthesizer is described in this report. Experimental design based on the knowledge obtained from previous screening experiments and the literature is the most effective initial step of the High‐Throughput Experimentation (HTE) cycle. In this paper, the polymerization procedure is explained step‐by‐step including preparation of stock solutions, inertization of the reactors and synthesizer environment, liquid transfers to or from the reactor vessels including sampling, as well as termination of the polymerization. Automated characterization techniques for the determination of monomer conversion and the molecular weight distribution of the polymers are discussed to complete the HTE cycle. Consequently, analysis of the data obtained from parallel screening of reactions and their products will result in the design of the next experimental cycle.