Reaction #324373

ord-d1355ead23f14183a85e53aeb6ff943a

Reaction equation

CCOCCOC(C)=O
ethylene glycol monoethyl ether acetate
COC(=O)C(C)(C)N=NC(C)(C)C(=O)OC
V-601
CCCCCC
hexane
C=C(C)C(=O)OC(C)(C)C.C=C(C)C(=O)OCc1ccccc1.C=Cc1ccc(OC(C)=O)cc1
4-acetoxystyrene t-butyl methacrylate benzyl methacrylate

Conditions

Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    Temperaturewas heated until the internal temperature of the flask
  2. 2
    Otherbecame 80° C
  3. 3
    workup.ADDITIONwas added
  4. 4
    workup.ADDITIONSubsequently, the above monomer mixture solution was dropped into this solution over a period of six hours
  5. 5
    TemperatureAfter the completion of the dropping, the mixture was further heated
  6. 6
    workup.STIRRINGagitated for two hours
  7. 7
    OtherThereafter, the reaction liquid
  8. 8
    OtherAfter the cooling, the reaction liquid
  9. 9
    Otherprecipitating a polymer
  10. 10
    FiltrationThe polymer solid was collected by filtration
  11. 11
    workup.DISSOLUTIONdissolved in 500 g of acetone
  12. 12
    workup.ADDITIONThis solution was dropped once more into three liters of hexane
  13. 13
    Filtrationthe thus obtained solid was collected by filtration
  14. 14
    Otherdried in vacuum

Procedure

The 2-liter flask charged with 600 g of ethylene glycol monoethyl ether acetate was heated until the internal temperature of the flask became 80° C. Then, 2.30 g (0.01 mol) of polymerization initiator V-601 was added thereto and agitated for five minutes. Subsequently, the above monomer mixture solution was dropped into this solution over a period of six hours. After the completion of the dropping, the mixture was further heated and agitated for two hours. Thereafter, the reaction liquid was cooled to room temperature. After the cooling, the reaction liquid was dropped into three liters of hexane, thereby precipitating a polymer. The polymer solid was collected by filtration and dissolved in 500 g of acetone. This solution was dropped once more into three liters of hexane, and the thus obtained solid was collected by filtration and dried in vacuum. Thus, 151 g of poly(4-acetoxystyrene/t-butyl methacrylate/benzyl methacrylate) was obtained.

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08642245B2uspto-grants-2014_02