"Reactive filtration": Use of functionalized porous polymer monoliths as scavengers in solution-phase synthesis

Organic Letters

Volumn 2, Issue 2, 2000, Pages 195-198

  Tripp, Jennifer A ^a   Stein, Jason A ^a   Svec, Frantisek ^a   Fréchet, Jean M J ^a  

^a UNIVERSITY OF CALIFORNIA   (United States)

Author keywords

[No Author keywords available]

Indexed keywords

POLYMER; SCAVENGER;

ARTICLE; CHEMISTRY; SOLUTION AND SOLUBILITY; SYNTHESIS;

CHEMISTRY; FREE RADICAL SCAVENGERS; POLYMERS; SOLUTIONS;

EID: 0034719269     PISSN: 15237060     EISSN: None     Source Type: Journal    
DOI: 10.1021/ol9912837     Document Type: Article

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35. Preparation of Macroporous Poly(chloromethylstyrene-co-divinylbenzene) Monolith. A mold consisting of a glass tube sealed at one end and containing shrinkable PE tube is filled with a solution of 0.12 g of azobisisobutyronitrile in chloromethylstyrene (4.8 g), divinylbenzene (tech grade, 7.2 g), toluene (5.25 g), and 1-dodecanol (12.75 g), and the open end of the mold is sealed using a proper size rubber septum secured with wire and electrical tape. The polymerization is achieved by heating the mold to 70 °C for 20 h. The glass tube is carefully broken, and the monoliths are sliced using a table saw and cleaned by THF extraction in a Soxhlet apparatus. The mean pore diameter of this monolith as determined by mercury porosimetry is 1.2 μm.
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38. Preparation of Macroporous Poly(4-vinyl-2,2-dimethylazlactone-co-ethylene dimethacrylate) Monolith. The poly(4-vinyl-2,2-dimethylazlactone-co-ethylene dimethacrylate) monolith is prepared in the same mold as described above. A solution of 0.24 g of azobisisobutyronitrile in 4-vinyl-2,2-dimethylazlactone (0.33 g), acrylamide (0.24 g), styrene (0.63 g), ethylene dimethacrylate (1.2 g), and 1-tetradecanol (3.6 g) is polymerized at 65 °C for 20 h. The workup and the preparation of the discs is identical with the other procedure.