Reaktion #2146714

ord-47bd86735c44470298473cbb422792dd

Reaktionsgleichung

CCOC(=O)OCC
diethyl carbonate
CC(C)(C#N)N=NC(C)(C)C#N
2,2′-azobis(isobutyronitrile)
C=C(C)C(=O)OC
methyl methacrylate
C=C(C)C(=O)OCC1(CC)COC1
3-ethyl-3-oxetanylmethyl methacrylate
C=CC(=O)OCC1CCC2OC2C1
3,4-epoxycyclohexylmethyl acrylate
O=C1OCCO1
ethylene carbonate
CC(C)(C#N)N=NC(C)(C)C#N
2,2′-azobis(isobutyronitrile)
CCOC(=O)OCC.O=C1OCCO1
ethylene carbonate diethyl carbonate

Reaktionsbedingungen

Temperatur
70°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeequipped with a refluxing condenser
  2. 2
    workup.ADDITIONmixed for 30 minutes while nitrogen gas
  3. 3
    workup.ADDITIONwas introduced into the flask
  4. 4
    Sonstigeradical polymerization
  5. 5
    SonstigeThe resulting reaction mixture
  6. 6
    Temperaturwas cooled to 40° C
  7. 7
    Temperaturthe resulting mixture was again heated to 70° C.
  8. 8
    Sonstigepolymerization at the temperature for another 8 hours
  9. 9
    SonstigeThen the resulting reaction mixture
  10. 10
    Temperaturwas cooled to 40° C.

Vorschrift

60.0 g of methyl methacrylate, 16.0 g of 3-ethyl-3-oxetanylmethyl methacrylate, 4.0 g of 3,4-epoxycyclohexylmethyl acrylate, 226.6 g of ethylene carbonate and 0.15 g 2,2′-azobis(isobutyronitrile) were placed in a 500 mL capacity three-necked flask equipped with a refluxing condenser and stirred and mixed for 30 minutes while nitrogen gas was introduced into the flask. Then the resulting mixture was heated to 70° C. and radical polymerization was carried out over 8 hours at the temperature. The resulting reaction mixture was cooled to 40° C. 226.6 g of diethyl carbonate and 0.15 g of 2,2′-azobis(isobutyronitrile) were added to the reaction mixture and the resulting mixture was again heated to 70° C. to carry out radical polymerization at the temperature for another 8 hours. Then the resulting reaction mixture was cooled to 40° C. to obtain a solution of a polymer in a concentration of 15% by weight in a solvent of ethylene carbonate/diethyl carbonate mixture.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08277897B2uspto-grants-2012_10