Chemicals and reagents
Chemicals and reagents
1 All reagents were purchased from Sigma-Aldrich and used without further purification unless specified
Synthesis of ChloroSMA20
Synthesis of ChloroSMA20
2 To a Amount 50 mL round bottom flask add Concentration 1.52 millimolar (mM) chloro-styrene , Concentration 1.52 millimolar (mM) maleic anhydride , and Concentration 0.076 millimolar (mM) 2-(dodecylthiocarbonothioylthio) propionic acid .
3 Dissolve in dimethylformamide.
4 Add Concentration 0.004 millimolar (mM) 1,1-Azobis(cyclohexanecarbonitrile) .
5 Cap the flask with a rubber stopper and bubble with nitrogen for Duration 00:15:00 minutes.
6 Heat to Temperature 90 °C for Duration 16:00:00 hours.
7 Precipitate in isopropanol or water, filter, and dry in vacuo.
Synthesis of ChloroSMA 40
Synthesis of ChloroSMA 40
8 To a Amount 50 mL round bottom flask add Concentration 3.1 millimolar (mM) chloro-styrene , Concentration 3.1 millimolar (mM) maleic anhydride , and Concentration 0.076 millimolar (mM) 2-(dodecylthiocarbonothioylthio) propionic acid .
9 Dissolve in dimethylformamide.
10 Add Concentration 0.004 millimolar (mM) 1,1-Azobis(cyclohexanecarbonitrile) .
11 Cap the flask with a rubber stopper and bubble with nitrogen for Duration 00:15:00 minutes.
12 Heat to Temperature 90 °C for Duration 16:00:00 hours.
13 Precipitate in isopropanol or water, filter, and dry in vacuo.
Synthesis of ChloroSMA 60
Synthesis of ChloroSMA 60
14 To a Amount 50 mL round bottom flask add Concentration 4.56 millimolar (mM) chloro-styrene , Concentration 4.56 millimolar (mM) maleic anhydride , and Concentration 0.076 millimolar (mM) 2-(dodecylthiocarbonothioylthio) propionic acid .
15 Dissolve in dimethylformamide.
16 Add Concentration 0.004 millimolar (mM) 1,1-Azobis(cyclohexanecarbonitrile) .
17 Cap the flask with a rubber stopper and bubble with nitrogen for Duration 00:15:00 minutes.
18 Heat to Temperature 90 °C for Duration 16:00:00 hours.
19 Precipitate in isopropanol or water, filter, and dry in vacuo.
Synthesis of ChloroSMA 80
Synthesis of ChloroSMA 80
20 To a Amount 50 mL round bottom flask add Concentration 6.1 millimolar (mM) chloro-styrene , Concentration 6.1 millimolar (mM) maleic anhydride , and Concentration 0.076 millimolar (mM) 2-(dodecylthiocarbonothioylthio) propionic acid .
21 Dissolve in dimethylformamide.
22 Add Concentration 0.004 millimolar (mM) 1,1-Azobis(cyclohexanecarbonitrile) .
23 Cap the flask with a rubber stopper and bubble with nitrogen for Duration 00:15:00 minutes.
24 Heat to Temperature 90 °C for Duration 16:00:00 hours.
25 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
26 Dissolve precipitated polymer in dimethylformamide and add Concentration 9.9 millimolar (mM) benzoyl peroxide to a round bottom flask.
27 Seal with a rubber stopper and bubble with nitrogen for Duration 00:15:00 minutes.
28 Leave the escape needle in the flask and heat to Temperature 90 °C for Duration 06:00:00 hours.
29 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)
30 In a round bottom flask dissolve Amount 800 mg anhydride polymer in Amount 2 g KOH and Amount 20 mL water .
31 Reflux for Duration 04:00:00 hours. The mixture should become clear.
32 Dialyze the hydrolyzed polymer using a 3.5KDa mwco membrane for Duration 36:00:00 hours.
33 Add water to precipitate the polymer.
34 Wash polymer using 0.1N HCl, 3 times, and dry the polymer under nitrogen.