Oxygen → styrene N-cyclohexyl maleimide

HRID 1264141노트

반응식

HRID 1264141 반응식
[CH2:1]=[CH:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[CH:9]1([N:15]2[C:19](=[O:20])[CH:18]=[CH:17][C:16]2=[O:21])[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]1.CCCCC(C1C=CN=C(C2C=C(C(CCCC)CCCC)C=CN=2)C=1)CCCC.C1(C(Br)C)C=CC=CC=1.O=O>>[CH2:1]=[CH:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[CH:9]1([N:15]2[C:19](=[O:20])[CH:18]=[CH:17][C:16]2=[O:21])[CH2:10][CH2:11][CH2:12][CH2:13][CH2:14]1

참가 물질

6

반응물 5

HCID 977OxygenHCID 7501StyreneHCID 11454(1-Bromoethyl)benzeneHCID 742031H-Pyrrole-2,5-dione, 1-cyclohexyl-HCID 1749844,4'-Bis(1-butylpentyl)-2,2'-bipyridine

생성물 1

HCID 86758900styrene N-cyclohexyl maleimide

실험 절차

The following amounts of reagents were weighed into glass tube under ambient temperature: 12 mg (8.37×10−2 mmol) of CuBr, 0.45 mL (0.41 g, 4.4 mmol) of deinhibited styrene, 0.72 g (4.4 mmol) N-cyclohexyl maleimide, 60 mg (0.175 mmol) 4,4′-di-(5-nonyl)-2,2′-bipyridine, and 12 μL (8.8×10−2 mmol) 1-phenylethyl bromide. Two “freeze-pump-thaw” cycles were performed on the content of tube in order to ensure that oxygen was removed from the polymerization solution. The tube was sealed under vacuum and placed in an oil bath thermostated at 110° C. After 7 h the tube was broken and the contents dissolved in 10 mL of THF. Conversion of the monomer, measured using GC was 98% for both monomers, and the molecular weight and polydispersity measured by GPC were Mn=4700, and Mw/Mn=1.22. From 1H NMR spectrum the content of styrene in copolymer was 50%. DSC measurement showed one Tg=270° C. The initial temperature of decomposition of the alternating copolymer determined from TGA was 430° C.

후처리

  1. customThe following amounts of reagents were weighed into glass tube under ambient temperature
  2. customTwo “freeze-pump-thaw” cycles were performed on the content of tube in order
  3. customwas removed from the polymerization solution
  4. customThe tube was sealed under vacuum
  5. customplaced in an oil bath
  6. customat 110° C
  7. dissolutionthe contents dissolved in 10 mL of THF
  8. customwas 430° C.

출처 및 근거

ORD 기록
ord-251a36f86e764ab3851f2691a90fc6cc
출처 데이터셋
uspto-grants-2003_04
특허 번호
US06541580B1

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