反应 #487492

ord-5a686f19aa234179b72d9ccdf8179a8f

反应方程式

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
收率 162.8%

反应条件

温度
72°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他To a 1000-ml three-neck flask equipped with a stirrer and a condenser
  2. 2
    其他To 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
    其他to react for an additional one hour
  6. 6
    其他a solution prepared
  7. 7
    workup.ADDITIONwas added
  8. 8
    温度The temperature of the mixture was raised to 78° C.
  9. 9
    温度the mixture was heated for 4 hours
  10. 10
    其他The resulting reaction solution
  11. 11
    其他was subjected to re-precipitation twice with an excess amount of hexane
  12. 12
    其他the precipitated resin was dried

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08740369B2uspto-grants-2014_06