Mwm Martin Fijten

Microwave-assisted synthesis and properties of a series of poly(2-alkyl-2-oxazoline)s

Microwave-assisted organic synthesis is a quickly expanding field of research. The fast non-contact (super)heating of the reaction mixtures has already resulted in many examples of increased reaction rates and improved yields. However, the number of investigations focusing on microwave-assisted polymerizations, and especially living/controlled polymerizations, is still limited. Following our recent success in accelerating the cationic ring-opening polymerization of 2-oxazolines, we report here our studies on the cationic polymerization of a series of linear 2-alkyl-2-oxazolines under microwave irradiation. The effect of chain length on the polymerization kinetics was investigated. Moreover, the microwave polymerization of 2-ethyl-2-oxazoline was further investigated by 1H-NMR spectroscopy to determine the active species during the polymerization. Besides the microwave polymerization of the linear 2-alkyl-2-oxazoline monomers, the thermal and surface properties of the resulting polymers were investigated by DSC and contact-angle measurements to study the effect of side-chain length on the polymer properties.

Star-shaped Poly(2-oxazoline)s by Dendrimer Endcapping

The synthesis of star-shaped poly(2-ethyl-2-oxazoline) is reported by direct end-capping of the living polymer chains with dendritic multiamines. The end-capping kinetics after addition of a first generation polypropylenimine dendrimer are discussed based on monitoring by size exclusion chromatography, revealing less efficient end-capping with larger poly(2-ethyl-2-oxazoline) chains and increasing dendrimer generation. In addition, it is demonstrated that the solution viscosity and cloud point temperature of the star-shaped polymers are much less affected by chain length compared with their linear analogues.

High-throughput experimentation applied to atom transfer radical polymerization: Automated optimization of the copper catalysts removal from polymers

Abstract Combinatorial chemistry and high-throughput experimentation have drawn great attention in recent years because of their significant advantages in increasing the research productivity. One of the emerging fields is their application in polymer science. Herein we describe the high-throughput optimization of purification conditions for polymers prepared via atom transfer radical polymerization using an automated synthesizer. The effects of the column materials, column lengths and eluent volumes on the purification efficiency as well as the molecular weights of the obtained purified polymers were systematically investigated for the first time. The optimum purification conditions for the removal of copper catalysts are provided. As a result an online high-throughput purification workflow using SPE cartridges is now available for the utilization in automated parallel synthesizers for ATRP screening experiment.