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Propylene → Propylene Vinylethylene Carbonate

HRID 2288944
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HRID 2288944 반응식
[CH2:1]=[CH:2][CH3:3].[C:4](=[O:7])([OH:6])[OH:5].[CH:8]([CH:10]=[CH2:11])=[CH2:9]>>[CH2:1]=[CH:2][CH3:3].[C:4]1(=[O:6])[O:5][CH2:11][CH:10]([CH:8]=[CH2:9])[O:7]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 8252PropyleneHCID 56924127Buta-1,3-diene;carbonic acid

생성물 1

HCID 86755543Propylene Vinylethylene Carbonate

반응 조건

온도
23 °C

실험 절차

A 200 mL flame dried pear-shaped Schlenk flask equipped with a magnetic stir bar and capped with a septum was charged with (2,6-di-isopropylphenylimino)-1,4-dithiane Pd(II) catalyst XII (100 mg) in an argon filled glove box. Upon removal from the glove box, the flask was evacuated and backfilled with propylene. The catalyst was dissolved in CH2Cl2 (20 mL) and immediately treated with vinyl ethylene carbonate (5 mL). The resulting orange solution was stirred at 23° C. under a propylene 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 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 2 days to afford a tacky solid (0.8 g, 284 TO). 1H NMR was consistent with a copolymer containing approximately 91.9 weight % propylene and 8.1 weight % vinyl ethylene carbonate monomer units.; Mn 4000 g /mol ; Mw 8110 g /mol.

후처리

  1. temperatureA 200 mL flame dried pear-shaped Schlenk flask
  2. customequipped with a magnetic stir bar
  3. customcapped with a septum
  4. customUpon removal from the glove box
  5. customthe flask was evacuated
  6. dissolutionThe catalyst was dissolved in CH2Cl2 (20 mL)
  7. additionimmediately treated with vinyl ethylene carbonate (5 mL)
  8. customA small amount of polymer had precipitated out of solution
  9. customThe polymerization was quenched with MeOH and acetone leaving oil adhering to the walls of the flask
  10. washThe polymer was washed several times with acetone and MeOH
  11. customto remove any remaining monomer
  12. dissolutionThe polymer was dissolved in CH2Cl2
  13. waitThe solvent was left
  14. customto evaporate
  15. customthe resulting oily polymer was dried in vacuo at ~80° C. for 2 days
  16. customto afford a tacky solid (0.8 g, 284 TO)

출처 및 근거

ORD 기록
ord-8a628d8b3b5844de8be5dbec59377e73
출처 데이터셋
uspto-grants-2000_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06090900

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