HRID2288942

反应详情

EQUATION

反应方程式

HRID 2288942 的结构方程式

CONDITIONS

反应条件

温度
23 °C

PROCEDURE

实验过程

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.

WORKUP

后处理

  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.