Dichloromethane → HCID 86658589, compound

HRID 2207856Notes

Reaction equation

HRID 2207856 reaction equation
C(Cl)Cl.[C:4]([O:8][CH3:9])(=[O:7])[CH:5]=[CH2:6].C=CC>C1(C)C=CC=CC=1>[CH2:4]=[CH:5][CH3:6].[C:4]([O:8][CH3:9])(=[O:7])[CH:5]=[CH2:6]

Participants

5

Procedure

Methylene chloride slurries (0.02 mol/L) of bis(benzylideneacetone)palladium and Phosphorus-Sulfonic Acid Ligand (I) were separately prepared and after treatment by an ultrasonic vibrator, mixed in a molar ratio of 1:1, and the mixture was stirred at room temperature for 15 minutes. Subsequently, the 10 mL stainless autoclave reactor was purged with purified nitrogen, and purified toluene and methyl acrylate (6 mmol) were introduced. After raising the temperature to 80° C. and pressurizing the system with propylene to 0.5 MPa, 8 μmol of the catalyst slurry prepared above was added, and polymerization was started. Here, the total liquid amount was adjusted to become 5 mL during the polymerization. The temperature was kept constant during the reaction, and propylene was continuously supplied so that the partial pressure of propylene could be kept at 0.5 MPa. After 60 minutes, the unreacted propylene was purged, and the autoclave was cooled to room temperature. The entire amount of the solvent was removed by evaporation, and the polymer was dried under reduced pressure at 40° C. for 6 hours and recovered. The catalytic activity was 3.90E+03 g/mol/h. The molecular weight Mw of the obtained polymer was 194,000 in terms of polyethylene, and Mw/Mn was 2.0.

Workup

  1. additionafter treatment by an ultrasonic vibrator, mixed in a molar ratio of 1:1
  2. customSubsequently, the 10 mL stainless autoclave reactor was purged with purified nitrogen
  3. additionwere introduced
  4. temperatureAfter raising the temperature to 80° C.
  5. customprepared
  6. additionabove was added
  7. custompolymerization
  8. customduring the polymerization
  9. waitAfter 60 minutes
  10. customthe unreacted propylene was purged
  11. temperaturethe autoclave was cooled to room temperature
  12. customThe entire amount of the solvent was removed by evaporation
  13. customthe polymer was dried under reduced pressure at 40° C. for 6 hours
  14. customrecovered

Sources & evidence

ORD record
ord-7891061b308642c992c02319df7e87b1
Source dataset
uspto-grants-2016_06
Patent number
US09376459B2

Reaction notes

Loading…