Methacrylic Acid → Phenoxyethylmethacrylate methylmethacrylate methacrylic acid

HRID 400309

反応式

HRID 400309 の反応式
[C:1]([O:6][CH2:7][CH2:8][O:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)(=[O:5])[C:2]([CH3:4])=[CH2:3].[C:16]([OH:21])(=[O:20])[C:17]([CH3:19])=[CH2:18].[C:22]([O:27][CH3:28])(=[O:26])[C:23]([CH3:25])=[CH2:24]>C(C(C)=O)C.COC(=O)C(N=NC(C)(C)C(OC)=O)(C)C>[C:1]([O:6][CH2:7][CH2:8][O:9][C:10]1[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=1)(=[O:5])[C:2]([CH3:4])=[CH2:3].[C:22]([O:27][CH3:28])(=[O:26])[C:23]([CH3:25])=[CH2:24].[C:16]([OH:21])(=[O:20])[C:17]([CH3:19])=[CH2:18]

参加物

6

反応物 3

HCID 4093Methacrylic AcidHCID 6658Methyl MethacrylateHCID 663572-Phenoxyethyl methacrylate

生成物 1

HCID 67403649Phenoxyethylmethacrylate methylmethacrylate methacrylic acid収率 162.8%

試薬・触媒・溶媒 2

HCID 757631,1'-Dimethyl 2,2'-(1,2-diazenediyl)bis(2-methylpropanoate)触媒2 回HCID 6569Methyl Ethyl Ketone溶媒3 回

反応条件

温度
72 °C

実験手順

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.

後処理

  1. customTo a 1,000-ml three-neck flask equipped with a stirrer and a condenser
  2. customTo this flask, a solution, prepared
  3. additionwas added dropwise over 3 hours
  4. additionAfter the completion of the dropwise addition
  5. customto react for an additional one hour
  6. customa solution prepared
  7. additionwas added
  8. temperatureThe temperature of the mixture was raised to 78° C.
  9. temperaturethe mixture was heated for 4 hours
  10. customThe resulting reaction solution
  11. customwas subjected to re-precipitation twice with an excess amount of hexane
  12. customthe precipitated resin was dried

出典と根拠

ORDレコード
ord-b0940d495828445aac3d2b7385a3e14e
出典データセット
uspto-grants-2014_06
特許番号
US08740369B2

関連ノート

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