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Ethylene → Ethylene Vinylethylene Carbonate

HRID 2288942
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HRID 2288942 반응식
C=C.[C:3](=[O:6])([OH:5])[OH:4].[CH:7]([CH:9]=[CH2:10])=[CH2:8]>>[CH2:7]=[CH2:8].[C:3]1(=[O:5])[O:4][CH2:10][CH:9]([CH:7]=[CH2:8])[O:6]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 6325EthyleneHCID 56924127Buta-1,3-diene;carbonic acid

생성물 1

HCID 86755542Ethylene Vinylethylene Carbonate

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온도
23 °C

실험 절차

Upon removal from the glove box, the flask was evacuated and backfilled with ethylene. The catalyst was dissolved in CH2Cl2 (25 mL) and immediately treated with vinyl ethylene carbonate (5 mL). The resulting orange solution was stirred at 23° C. under an ethylene atmosphere (1 atm) for 20 hours. A small amount of polymer had precipitated out of solution. The polymerization was quenched with MeOH and acetone leaving gray oil adhering to the walls of the flask. The polymer was washed several times with acetone and MeOH to remove any remaining monomer. The polymer was dissolved in CH2Cl2 and transferred to a storage jar. The solvent was left to evaporate and the resulting oily polymer was dried in vacuo at ~80° C. for 3 days to afford a tacky solid (2.15 g, 1100 TO). 1H NMR was consistent with a copolymer containing approximately 96.5 weight % ethylene and 3.5 weight % vinyl ethylene carbonate monomer units.; Mn 40,000 g /mol ; Mw 92,000 g /mol ; DSC Tg -68° C., Tm -38° C.

후처리

  1. customUpon removal from the glove box
  2. customthe flask was evacuated
  3. dissolutionThe catalyst was dissolved in CH2Cl2 (25 mL)
  4. additionimmediately treated with vinyl ethylene carbonate (5 mL)
  5. customA small amount of polymer had precipitated out of solution
  6. customThe polymerization was quenched with MeOH and acetone leaving gray oil adhering to the walls of the flask
  7. washThe polymer was washed several times with acetone and MeOH
  8. customto remove any remaining monomer
  9. dissolutionThe polymer was dissolved in CH2Cl2
  10. waitThe solvent was left
  11. customto evaporate
  12. customthe resulting oily polymer was dried in vacuo at ~80° C. for 3 days
  13. customto afford a tacky solid (2.15 g, 1100 TO)
  14. customDSC Tg -68° C., Tm -38° C.

출처 및 근거

ORD 기록
ord-6e03554d938c40939e9e43ff58be5b76
출처 데이터셋
uspto-grants-2000_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06090900

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