May 04, 2024

Public workspaceRAFT Based Synthesis of In-house Polymers

DOI
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: 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
Abstract
The protocol gives details for synthesizing the ChloroSMA series of membrane active polymers.
Chemicals and reagents
Chemicals and reagents
All reagents were purchased from Sigma-Aldrich and used without further purification unless specified 
otherwise. 
Synthesis of ChloroSMA20
Synthesis of ChloroSMA20
To a Amount50 mL round bottom flask add Concentration1.52 millimolar (mM) chloro-styrene ,Concentration1.52 millimolar (mM) maleic anhydride , and Concentration0.076 millimolar (mM) 2-(dodecylthiocarbonothioylthio) propionic acid .

Dissolve in dimethylformamide.
Add Concentration0.004 millimolar (mM) 1,1-Azobis(cyclohexanecarbonitrile) .
Cap the flask with a rubber stopper and bubble with nitrogen for Duration00:15:00 minutes.

15m
Heat to Temperature90 °C for Duration16:00:00 hours.

16h
Precipitate in isopropanol or water, filter, and dry in vacuo.
Synthesis of ChloroSMA 40
Synthesis of ChloroSMA 40
16h 15m
16h 15m
To a Amount50 mL round bottom flask add Concentration3.1 millimolar (mM) chloro-styrene ,Concentration3.1 millimolar (mM) maleic anhydride , and Concentration0.076 millimolar (mM) 2-(dodecylthiocarbonothioylthio) propionic acid .


Dissolve in dimethylformamide.
Add Concentration0.004 millimolar (mM) 1,1-Azobis(cyclohexanecarbonitrile) .
Cap the flask with a rubber stopper and bubble with nitrogen for Duration00:15:00 minutes.
15m
Heat to Temperature90 °C for Duration16:00:00 hours.
16h
Precipitate in isopropanol or water, filter, and dry in vacuo.
Synthesis of ChloroSMA 60
Synthesis of ChloroSMA 60
16h 15m
16h 15m
To a Amount50 mL round bottom flask add Concentration4.56 millimolar (mM) chloro-styrene ,Concentration4.56 millimolar (mM) maleic anhydride , and Concentration0.076 millimolar (mM) 2-(dodecylthiocarbonothioylthio) propionic acid .

Dissolve in dimethylformamide.
Add Concentration0.004 millimolar (mM) 1,1-Azobis(cyclohexanecarbonitrile) .
Cap the flask with a rubber stopper and bubble with nitrogen for Duration00:15:00 minutes.

15m
Heat to Temperature90 °C for Duration16:00:00 hours.
16h
Precipitate in isopropanol or water, filter, and dry in vacuo.
Synthesis of ChloroSMA 80
Synthesis of ChloroSMA 80
16h 15m
16h 15m
To a Amount50 mL round bottom flask add Concentration6.1 millimolar (mM) chloro-styrene ,Concentration6.1 millimolar (mM) maleic anhydride , and Concentration0.076 millimolar (mM) 2-(dodecylthiocarbonothioylthio) propionic acid .
Dissolve in dimethylformamide.
Add Concentration0.004 millimolar (mM) 1,1-Azobis(cyclohexanecarbonitrile) .
Cap the flask with a rubber stopper and bubble with nitrogen for Duration00:15:00 minutes.

15m
Heat to Temperature90 °C for Duration16:00:00 hours.
16h
Precipitate in isopropanol or water, filter, and dry in vacuo.
End-group removal of poly(4 chlorostyrene-alt-maleic anhydride
End-group removal of poly(4 chlorostyrene-alt-maleic anhydride
6h 15m
6h 15m
Dissolve precipitated polymer in dimethylformamide and add Concentration9.9 millimolar (mM) benzoyl peroxide to a round bottom flask.

Seal with a rubber stopper and bubble with nitrogen for Duration00:15:00 minutes.

15m
Leave the escape needle in the flask and heat to Temperature90 °C for Duration06:00:00 hours.

6h
Precipitate polymer with isopropanol or water and dry in vacuo.
Hydrolysis to produce poly(4 chlorostyrene-alt-maleic acid)
Hydrolysis to produce poly(4 chlorostyrene-alt-maleic acid)
1d 16h
1d 16h
In a round bottom flask dissolve Amount800 mg anhydride polymer in Amount2 g KOH and Amount20 mL water .

Reflux for Duration04:00:00 hours. The mixture should become clear.

4h
Dialyze the hydrolyzed polymer using a 3.5KDa mwco membrane for Duration36:00:00 hours.

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