RAFT Based Synthesis of In-house Polymers
Caroline Brown, Snehasish Ghosh, Kallol Gupta
Abstract
The protocol gives details for synthesizing the ChloroSMA series of membrane active polymers.
Steps
Chemicals and reagents
All reagents were purchased from Sigma-Aldrich and used without further purification unless specified
otherwise.
Synthesis of ChloroSMA20
To a 50mL add 1.52millimolar (mM) ,1.52millimolar (mM) , and 0.076millimolar (mM) .
Dissolve in dimethylformamide.
Add 0.004millimolar (mM) .
Cap the flask with a rubber stopper and bubble with nitrogen for 0h 15m 0s minutes.
Heat to 90°C for 16h 0m 0s hours.
Precipitate in isopropanol or water, filter, and dry in vacuo.
Synthesis of ChloroSMA 40
To a 50mL add 3.1millimolar (mM) ,3.1millimolar (mM) , and 0.076millimolar (mM).
Dissolve in dimethylformamide.
Add 0.004millimolar (mM) .
Cap the flask with a rubber stopper and bubble with nitrogen for 0h 15m 0s minutes.
Heat to 90°C for 16h 0m 0s hours.
Precipitate in isopropanol or water, filter, and dry in vacuo.
Synthesis of ChloroSMA 60
To a 50mL add 4.56millimolar (mM) ,4.56millimolar (mM) , and 0.076millimolar (mM) .
Dissolve in dimethylformamide.
Add 0.004millimolar (mM) .
Cap the flask with a rubber stopper and bubble with nitrogen for 0h 15m 0s minutes.
Heat to 90°C for 16h 0m 0s hours.
Precipitate in isopropanol or water, filter, and dry in vacuo.
Synthesis of ChloroSMA 80
To a 50mL add 6.1millimolar (mM) ,6.1millimolar (mM) , and 0.076millimolar (mM) .
Dissolve in dimethylformamide.
Add 0.004millimolar (mM) .
Cap the flask with a rubber stopper and bubble with nitrogen for 0h 15m 0s minutes.
Heat to 90°C for 16h 0m 0s hours.
Precipitate in isopropanol or water, filter, and dry in vacuo.
End-group removal of poly(4 chlorostyrene-alt-maleic anhydride
Dissolve precipitated polymer in dimethylformamide and add 9.9millimolar (mM) to a round bottom flask.
Seal with a rubber stopper and bubble with nitrogen for 0h 15m 0s minutes.
Leave the escape needle in the flask and heat to 90°C for 6h 0m 0s hours.
Precipitate polymer with isopropanol or water and dry in vacuo.
Hydrolysis to produce poly(4 chlorostyrene-alt-maleic acid)
In a round bottom flask dissolve 800mg in 2g and 20mL.
Reflux for 4h 0m 0s hours. The mixture should become clear.
Dialyze the hydrolyzed polymer using a 3.5KDa mwco membrane for 36h 0m 0s hours.
Add water to precipitate the polymer.
Wash polymer using 0.1N HCl, 3 times, and dry the polymer under nitrogen.
