The Library
Data for High-throughput tertiary amine deoxygenated photopolymerizations for synthesizing polymer libraries
Tools
Stubbs, Christopher D., Congdon, Thomas R., Davis, Jessica, Lester, Daniel, Richards, Sarah-Jane and Gibson, Matthew I. (2019) Data for High-throughput tertiary amine deoxygenated photopolymerizations for synthesizing polymer libraries. [Dataset]
Plain Text (Readme file)
Directory.txt - Published Version Available under License Creative Commons Attribution 4.0. Download (533b) |
|
Archive (ZIP) (Experimental data)
WRAP data.zip - Published Version Available under License Creative Commons Attribution 4.0. Download (5Mb) |
Official URL: http://wrap.warwick.ac.uk/128153
Abstract
The huge chemical space potential of synthetic polymers means that in many studies only a small parameter range can be realistically synthesized in a short time and hence the “best” formulations may not be optimum. Throughput is traditionally limited by the need for deoxygenation in radical polymerizations, but advances in photopolymerization now provide opportunities for “in-air” polymerizations. Here, we have developed a protocol using liquid handling robots (or multichannel pipettes) with blue light photolysis of reversible addition fragmentation chain transfer agents and tertiary amine deoxygenation to enable the synthesis of polymer libraries in industry-standard 96-well plates with no specialized infrastructure and no degassing step. The roles of solvents and amine deoxygenators are explored to optimize the polymerization, particularly to look at alternatives to dimethyl sulfoxide (DMSO) for hydrophobic monomer (co)polymerization. DMSO is shown to aid the degassing process but is not easy to remove and hence prevents isolation of pure polymers. In contrast, using dioxane in-plate evaporation or precipitation of the tertiary amine allowed isolation of polymers in-plate. This removed all reaction components yielding pure polymers, which is not easily achieved with systems using metal catalysts and secondary reductants, such as ascorbic acid. As an example of the throughput, in just under 40 h, 392 polymers were synthesized and subsequently analyzed direct from plates by a 96-well plate sampling size exclusion chromatography system to demonstrate reproducibility. Due to less efficient degassing in dioxane (compared to DMSO), the molecular weight and dispersity control were limited in some cases (with acrylates giving the lowest dispersities), but the key aim of this system is to access hundreds of polymers quickly and in a format needed to enable testing. This method enables easy exploration of chemical space and development of screening libraries to identify hits for further study using precision polymerization methods.
Item Type: | Dataset | ||||||||||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
Subjects: | Q Science > QD Chemistry | ||||||||||||||||||
Divisions: | Faculty of Science, Engineering and Medicine > Science > Chemistry | ||||||||||||||||||
Type of Data: | Experimental data | ||||||||||||||||||
Library of Congress Subject Headings (LCSH): | Photopolymerization | ||||||||||||||||||
Journal or Publication Title: | Macromolecules | ||||||||||||||||||
Publisher: | University of Warwick, Department of Chemistry | ||||||||||||||||||
ISSN: | 0024-9297 | ||||||||||||||||||
Official Date: | 18 October 2019 | ||||||||||||||||||
Dates: |
|
||||||||||||||||||
DOI: | 10.1021/acs.macromol.9b01714 | ||||||||||||||||||
Status: | Not Peer Reviewed | ||||||||||||||||||
Publication Status: | Published | ||||||||||||||||||
Media of Output (format): | .csv .xlsx | ||||||||||||||||||
Access rights to Published version: | Open Access (Creative Commons) | ||||||||||||||||||
Copyright Holders: | University of Warwick | ||||||||||||||||||
Description: | WRAP data for High-Throughput Tertiary Amine De-oxygenated Photopolymerizations for |
||||||||||||||||||
Date of first compliant deposit: | 3 October 2019 | ||||||||||||||||||
Date of first compliant Open Access: | 3 October 2019 | ||||||||||||||||||
RIOXX Funder/Project Grant: |
|
||||||||||||||||||
Related URLs: | |||||||||||||||||||
Contributors: |
|
Request changes or add full text files to a record
Repository staff actions (login required)
View Item |
Downloads
Downloads per month over past year