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Volumn 49, Issue 50, 2008, Pages 7103-7105

Novel monodisperse PEG-grafted polystyrene resins: synthesis and application in gel-phase 13C NMR spectroscopy

Author keywords

NMR spectroscopy; PS PEG graft copolymers; Solid phase organic synthesis; TOF SIMS

Indexed keywords

COPOLYMER; MACROGOL; OLIGO(OXYETHYLENE); OLIGOMER; POLYSTYRENE; RESIN; UNCLASSIFIED DRUG;

EID: 54449094940     PISSN: 00404039     EISSN: None     Source Type: Journal    
DOI: 10.1016/j.tetlet.2008.09.128     Document Type: Article
Times cited : (3)

References (15)
  • 1
    • 54449098539 scopus 로고    scopus 로고
    • Bayer, E.; Hemmasi, B.; Albert, K.; Rapp, W.; Dengler, M. Peptides, Structure and Function. Hruby, V. J., Rich, D. H., Eds; Proceedings of the 8th American Peptide Symposium; Pierce Chemical Company: Rockford, IL, 1983; pp 87-90.
    • Bayer, E.; Hemmasi, B.; Albert, K.; Rapp, W.; Dengler, M. Peptides, Structure and Function. Hruby, V. J., Rich, D. H., Eds; Proceedings of the 8th American Peptide Symposium; Pierce Chemical Company: Rockford, IL, 1983; pp 87-90.
  • 7
    • 54449091734 scopus 로고    scopus 로고
    • note
    • 9Si: C, 54.52, H, 9.98. Found: C, 54.48, H, 9.72.
  • 8
    • 54449093469 scopus 로고    scopus 로고
    • note
    • Experimental procedure for Mitsunobu reaction on solid phase: Diethyl azodicarboxylate (5 equiv) was added dropwise to a mixture of 1.0 equiv of polymer-bounded phenol (100-200 mesh, 1% divinylbenzene, Aldrich, 1.7 mmol/g) in dry DCM/THF = 1/1 (50 mL/g resin) under argon. Then, the monoprotected glycol 2 (5 equiv), dissolved in dry THF, was added and finally triphenylphosphine was added slowly. The reaction mixture was stirred overnight, filtered, and the solid residue was washed three times with DCM/THF = 1/1, DCM, isopropanol, DCM and finally with methanol. The resulting resin 3 was dried to constant weight in vacuo.
  • 10
    • 54449088486 scopus 로고    scopus 로고
    • note
    • General procedure for preparation of resin 5: Resin 4 was suspended in dry DCM/DMF = 9/1 (15 mL/g resin), and then 4-(dimethylamino)-butyric acid hydrochloride (5.0 equiv) and 1-hydroxybenzotriazole (5.0 equiv) were added in a minimum amount of dry DMF. 4-(N,N-dimethylamino)-pyridine (1.0 equiv) in dry DMF and N,N′-diisopropylcarbodiimide (5.0 equiv.) were added to the mixture and were stirred under argon at room temperature for 2 days. The resulting suspension was filtered and the solid residue was washed three times with DMF, then with DCM, and finally with methanol. The resin was dried to constant weight in vacuo.
  • 12
    • 54449086132 scopus 로고    scopus 로고
    • note
    • 13
  • 13
    • 54449099172 scopus 로고    scopus 로고
    • note
    • The field of view is always 128 × 128 pixels, independent from the μm scale. The color scale depends on 'mc value' (maximum counts per pixel), not on the 'tc value' (total counts).


* 이 정보는 Elsevier사의 SCOPUS DB에서 KISTI가 분석하여 추출한 것입니다.