Reacción #487492

ord-5a686f19aa234179b72d9ccdf8179a8f

Ecuación de reacción

C=C(C)C(=O)OCCOc1ccccc1
phenoxyethyl methacrylate
C=C(C)C(=O)O
methacrylic acid
C=C(C)C(=O)OC
methyl methacrylate
C=C(C)C(=O)O.C=C(C)C(=O)OC.C=C(C)C(=O)OCCOc1ccccc1
phenoxyethyl methacrylate methyl methacrylate methacrylic acid
Rendimiento 162.8%

Condiciones de reacción

Temperatura
72°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    OtroTo a 1000-ml three-neck flask equipped with a stirrer and a condenser
  2. 2
    OtroTo this flask, a solution, prepared
  3. 3
    workup.ADDITIONwas added dropwise over 3 hours
  4. 4
    workup.ADDITIONAfter the completion of the dropwise addition
  5. 5
    Otroto react for an additional one hour
  6. 6
    Otroa solution prepared
  7. 7
    workup.ADDITIONwas added
  8. 8
    TemperaturaThe temperature of the mixture was raised to 78° C.
  9. 9
    Temperaturathe mixture was heated for 4 hours
  10. 10
    OtroThe resulting reaction solution
  11. 11
    Otrowas subjected to re-precipitation twice with an excess amount of hexane
  12. 12
    Otrothe precipitated resin was dried

Procedimiento

To a 1000-ml three-neck flask equipped with a stirrer and a condenser, 88 g of methyl ethyl ketone was added, and heated to 72° C. under a nitrogen atmosphere. To this flask, a solution, prepared by dissolving 0.85 g of dimethyl-2,2′-azobisisobutyrate, 50 g of phenoxyethyl methacrylate, 13 g of methacrylic acid and 37 g of methyl methacrylate in 50 g of methyl ethyl ketone, was added dropwise over 3 hours. After the completion of the dropwise addition, the content in the flask was allowed to react for an additional one hour, and then a solution prepared by dissolving 0.42 g of dimethyl-2,2′-azobisisobutyrate in 2 g of methyl ethyl ketone was added thereto. The temperature of the mixture was raised to 78° C., and the mixture was heated for 4 hours. The resulting reaction solution was subjected to re-precipitation twice with an excess amount of hexane, and the precipitated resin was dried. 96.5 g of a phenoxyethyl methacrylate/methyl methacrylate/methacrylic acid copolymer (resin dispersant P-1, copolymerization ratio by mass %=50/37/13) was thus obtained.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08740369B2uspto-grants-2014_06