Réaction #487491

ord-b0940d495828445aac3d2b7385a3e14e

Équation de réaction

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
Rendement 162.8%

Conditions de réaction

Température
72°CELSIUS
Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    AutreTo a 1,000-ml three-neck flask equipped with a stirrer and a condenser
  2. 2
    AutreTo 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
    Autreto react for an additional one hour
  6. 6
    Autrea solution prepared
  7. 7
    workup.ADDITIONwas added
  8. 8
    TempératureThe temperature of the mixture was raised to 78° C.
  9. 9
    Températurethe mixture was heated for 4 hours
  10. 10
    AutreThe resulting reaction solution
  11. 11
    Autrewas subjected to re-precipitation twice with an excess amount of hexane
  12. 12
    Autrethe precipitated resin was dried

Mode opératoire

To a 1,000-ml three-neck flask equipped with a stirrer and a condenser, 88 g of methyl ethyl ketone were 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 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 (copolymerization ratio by mass %=50/37/13) was thus obtained. This copolymer is referred to as water-insoluble resin P-2.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US08740369B2uspto-grants-2014_06