Controlled radical polymerization in the presence of oxygen

Macromolecules

Volumn 31, Issue 17, 1998, Pages 5967-5969

  Matyjaszewski, Krzysztof ^a   Coca, Simion ^a   Gaynor, Scott G ^a   Wei, Mingli ^a   Woodworth, Brian E ^a  

^a CARNEGIE MELLON UNIVERSITY   (United States)

Author keywords

[No Author keywords available]

Indexed keywords

BLOCK COPOLYMERS; CATALYSTS; COMPOSITION EFFECTS; COPPER COMPOUNDS; MOLECULAR STRUCTURE; MOLECULAR WEIGHT DISTRIBUTION; OXYGEN; POLYACRYLATES; POLYSTYRENES; REACTION KINETICS; SIZE EXCLUSION CHROMATOGRAPHY; SYNTHESIS (CHEMICAL);

ATOM TRANSFER RADICAL POLYMERIZATION (ATRP);

FREE RADICAL POLYMERIZATION;

EID: 0032137479     PISSN: 00249297     EISSN: None     Source Type: Journal    
DOI: 10.1021/ma9808528     Document Type: Article

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28. 2 (12 mg; 0.054 mmol), 4,4′-di(5-nonyl)-2,2′-bipyridine (107 mg; 0.262 mmol), 1-phenylethyl bromide (71.6 μL.; 0.525 mmol), and styrene (6 mL; 52.4 mmol) followed by 0.6 mL of chlorobenzene as an internal reference. All manipulations were performed in air. The styrene was unpurified and contained inhibitor (10-15 ppm 4-tertbutylcatechol). The sample vial was charged with a stir bar and then fitted with a rubber septum. The vial was then immersed in an oil bath and held by a thermostat at 110 °C with vigorous stirring. At various times, samples were taken via syringe and quenched with THF. The volume lost by sample removal was replaced with argon. The samples were used to monitor percent monomer conversion relative to the internal reference (GC) and molecular weight (SEC).
29. 2 (7.4 mg; 0.033 mmol), 4,4′-di(5-nonyl)-2,2′-bipyridine (68 mg; 0.166 mmol), methyl (±)-2-bromopropionate (37 μL; 0.33 mmol) and methyl acrylate (6 mL; 66.6 mmol) followed by 0.6 mL of chlorobenzene as an internal reference. All manipulations were performed in air. The methyl acrylate was unpurified and contained stabilizer (200 ppm hydroquinone monomethyl ether). The sample vial was charged with a stir bar and then fitted with a rubber septum. The vial was then immersed in an oil bath and held by a thermostat at 80 °C with vigorous stirring. At various times, samples were taken via syringe and quenched with THF. The volume lost by sample removal was replaced with argon. The samples were used to monitor percent monomer conversion relative to the internal reference (GC) and molecular weight (SEC).