May 04, 2024

RAFT Based Synthesis of In-house Polymers

DOI
https://dx.doi.org/10.17504/protocols.io.ewov19noylr2/v1
  • 1Nanobiology Institute, Yale University, West Haven, CT, USA;
  • 2Department of Cell Biology, Yale University School of Medicine, New Haven, CT, USA;
  • 3Aligning Science Across Parkinson’s (ASAP) Collaborative Research Network, Chevy Chase, MD, 20815
Caroline Brown
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DOI: https://dx.doi.org/10.17504/protocols.io.ewov19noylr2/v1
Protocol Citation: Caroline Brown, Snehasish Ghosh, Kallol Gupta 2024. RAFT Based Synthesis of In-house Polymers. protocols.io https://dx.doi.org/10.17504/protocols.io.ewov19noylr2/v1
License: This is an open access protocol distributed under the terms of the Creative Commons Attribution License,  which permits unrestricted use, distribution, and reproduction in any medium, provided the original author and source are credited
Protocol status: Working
We use this protocol and it's working
Created: May 03, 2024
Last Modified: May 04, 2024
Protocol Integer ID: 99193
Keywords: chlorosma series of membrane, chlorosma series, house polymer, active polymer, house polymers the protocol, membrane, synthesis of in, based synthesis
Abstract
The protocol gives details for synthesizing the ChloroSMA series of membrane active polymers.
Chemicals and reagents
All reagents were purchased from Sigma-Aldrich and used without further purification unless specified 
otherwise. 
Synthesis of ChloroSMA20
To a 50 mL round bottom flask add 1.52 millimolar (mM) chloro-styrene ,1.52 millimolar (mM) maleic anhydride , and 0.076 millimolar (mM) 2-(dodecylthiocarbonothioylthio) propionic acid .

Dissolve in dimethylformamide.
Add 0.004 millimolar (mM) 1,1-Azobis(cyclohexanecarbonitrile) .
Cap the flask with a rubber stopper and bubble with nitrogen for 00:15:00 minutes.

15m
Heat to 90 °C for 16:00:00 hours.

16h
Precipitate in isopropanol or water, filter, and dry in vacuo.
Synthesis of ChloroSMA 40
16h 15m
To a 50 mL round bottom flask add 3.1 millimolar (mM) chloro-styrene ,3.1 millimolar (mM) maleic anhydride , and 0.076 millimolar (mM) 2-(dodecylthiocarbonothioylthio) propionic acid .


Dissolve in dimethylformamide.
Add 0.004 millimolar (mM) 1,1-Azobis(cyclohexanecarbonitrile) .
Cap the flask with a rubber stopper and bubble with nitrogen for 00:15:00 minutes.
15m
Heat to 90 °C for 16:00:00 hours.
16h
Precipitate in isopropanol or water, filter, and dry in vacuo.
Synthesis of ChloroSMA 60
16h 15m
To a 50 mL round bottom flask add 4.56 millimolar (mM) chloro-styrene ,4.56 millimolar (mM) maleic anhydride , and 0.076 millimolar (mM) 2-(dodecylthiocarbonothioylthio) propionic acid .

Dissolve in dimethylformamide.
Add 0.004 millimolar (mM) 1,1-Azobis(cyclohexanecarbonitrile) .
Cap the flask with a rubber stopper and bubble with nitrogen for 00:15:00 minutes.

15m
Heat to 90 °C for 16:00:00 hours.
16h
Precipitate in isopropanol or water, filter, and dry in vacuo.
Synthesis of ChloroSMA 80
16h 15m
To a 50 mL round bottom flask add 6.1 millimolar (mM) chloro-styrene ,6.1 millimolar (mM) maleic anhydride , and 0.076 millimolar (mM) 2-(dodecylthiocarbonothioylthio) propionic acid .
Dissolve in dimethylformamide.
Add 0.004 millimolar (mM) 1,1-Azobis(cyclohexanecarbonitrile) .
Cap the flask with a rubber stopper and bubble with nitrogen for 00:15:00 minutes.

15m
Heat to 90 °C for 16:00:00 hours.
16h
Precipitate in isopropanol or water, filter, and dry in vacuo.
End-group removal of poly(4 chlorostyrene-alt-maleic anhydride
6h 15m
Dissolve precipitated polymer in dimethylformamide and add 9.9 millimolar (mM) benzoyl peroxide to a round bottom flask.

Seal with a rubber stopper and bubble with nitrogen for 00:15:00 minutes.

15m
Leave the escape needle in the flask and heat to 90 °C for 06:00:00 hours.

6h
Precipitate polymer with isopropanol or water and dry in vacuo.
Hydrolysis to produce poly(4 chlorostyrene-alt-maleic acid)
1d 16h
In a round bottom flask dissolve 800 mg anhydride polymer in 2 g KOH and 20 mL water .

Reflux for 04:00:00 hours. The mixture should become clear.

4h
Dialyze the hydrolyzed polymer using a 3.5KDa mwco membrane for 36:00:00 hours.

1d 12h
Add water to precipitate the polymer.
Wash polymer using 0.1N HCl, 3 times, and dry the polymer under nitrogen.