Azobisisobutyronitrile → Diethyl carbonate ethylene carbonate
Reaction equation
C(OC)(=O)C(C)=C.C(OCC1CCC2OC2C1)(=O)C=C.[C:21]1(=[O:26])[O:25][CH2:24][CH2:23][O:22]1.N(C(C)(C)C#N)=NC(C)(C)C#N.[C:39](=[O:46])([O:43][CH2:44][CH3:45])[O:40][CH2:41][CH3:42]>>[C:21]1(=[O:26])[O:25][CH2:24][CH2:23][O:22]1.[C:39](=[O:46])([O:43][CH2:44][CH3:45])[O:40][CH2:41][CH3:42]Participants
Conditions
- Temperature
- 70 °C
Procedure
60.0 g of methyl methacrylate, 20.0 g of 3,4-epoxycyclohexylmethyl acrylate, 226.6 g of ethylene carbonate and 0.24 g of 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. The mixture was heated to 70° C. and radical polymerization was carried out at the temperature over 8 hours. The resulting reaction mixture was cooled to 40° C. 226.6 g of diethyl carbonate and 0.24 g of 2,2′-azobis(isobutyronitrile) were added to the reaction mixture and the resulting mixture was again heated to 70° C. for carrying out radical polymerization at the temperature for another 8 hours. The resulting reaction mixture was cooled to 40° C. thereby to obtain a solution of a polymer in a concentration of 15% by weight in a solvent of ethylene carbonate/diethyl carbonate mixture.
Workup
- customequipped with a refluxing condenser
- additionmixed for 30 minutes while nitrogen gas
- additionwas introduced into the flask
- customradical polymerization
- customThe resulting reaction mixture
- temperaturewas cooled to 40° C
- temperaturethe resulting mixture was again heated to 70° C.
- custompolymerization at the temperature for another 8 hours
- customThe resulting reaction mixture
- temperaturewas cooled to 40° C.
Sources & evidence
- ORD record
- ord-0764a475bbd14958a0dfcc290f1a43c0
- Source dataset
- uspto-grants-2012_10
- Patent number
- US08277897B2
Reaction notes
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