Azobisisobutyronitrile → Diethyl carbonate ethylene carbonate

HRID 2059535Notes

Reaction equation

HRID 2059535 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.[C:40](=[O:47])([O:44][CH2:45][CH3:46])[O:41][CH2:42][CH3:43].N(C(C)(C)C#N)=NC(C)(C)C#N>>[C:34]1(=[O:39])[O:38][CH2:37][CH2:36][O:35]1.[C:40](=[O:47])([O:44][CH2:45][CH3:46])[O:41][CH2:42][CH3:43]

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 N,N′-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-55a59668d8d44351aca57b22bf4a9d6f
Source dataset
uspto-grants-2012_10
Patent number
US08277968B2

Reaction notes

Loading…