Azobisisobutyronitrile → Diethyl carbonate ethylene carbonate

HRID 2059532Notes

Reaction equation

HRID 2059532 reaction equation
C(OC)(=O)C(C)=C.C(OCC1(CC)COC1)(=O)C(C)=C.C(OCC1CCC2OC2C1)(=O)C=C.[C:34]1(=[O:39])[O:38][CH2:37][CH2:36][O:35]1.N(C(C)(C)C#N)=NC(C)(C)C#N.[C:52](=[O:59])([O:56][CH2:57][CH3:58])[O:53][CH2:54][CH3:55]>>[C:34]1(=[O:39])[O:38][CH2:37][CH2:36][O:35]1.[C:52](=[O:59])([O:56][CH2:57][CH3:58])[O:53][CH2:54][CH3:55]

Participants

7

Conditions

Temperature
70 °C

Procedure

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.

Workup

  1. customequipped with a refluxing condenser
  2. additionmixed for 30 minutes while nitrogen gas
  3. additionwas introduced into the flask
  4. customradical polymerization
  5. customThe resulting reaction mixture
  6. temperaturewas cooled to 40° C
  7. temperaturethe resulting mixture was again heated to 70° C.
  8. custompolymerization at the temperature for another 8 hours
  9. customThen the resulting reaction mixture
  10. temperaturewas cooled to 40° C.

Sources & evidence

ORD record
ord-47bd86735c44470298473cbb422792dd
Source dataset
uspto-grants-2012_10
Patent number
US08277897B2

Reaction notes

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