Methacrylic Acid → Phenoxyethylmethacrylate methylmethacrylate methacrylic acid

HRID 1471204

반응식

HRID 1471204 반응식
[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]>COC(=O)C(N=NC(C)(C)C(OC)=O)(C)C.C(C(C)=O)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]

참가 물질

6

반응물 3

HCID 4093Methacrylic AcidHCID 6658Methyl MethacrylateHCID 663572-Phenoxyethyl methacrylate

생성물 1

HCID 67403649Phenoxyethylmethacrylate methylmethacrylate methacrylic acid수율 162.8%

시약·촉매·용매 2

HCID 6569Methyl Ethyl Ketone용매3회HCID 757631,1'-Dimethyl 2,2'-(1,2-diazenediyl)bis(2-methylpropanoate)용매2회

반응 조건

온도
72 °C

실험 절차

88 g of methyl ethyl ketone was added to a 1000 ml three-necked flask that included a stirrer and condenser and heated in a nitrogen atmosphere to 72° C., and a solution in which 0.85 g of dimethyl-2,2′-azobisisobutyrate, 50 g of phenoxyethyl methacrylate, 13 g of methacrylic acid, and 37 g of methyl methacrylate were dissolved in 50 g of methyl ethyl ketone was added dropwise thereto over three hours. After reacting for another hour after the end of the dropwise addition, a solution in which 0.42 g of dimethyl-2,2′-azobisisobutyrate was dissolved in 2 g of methyl ethyl ketone was added, heated to and maintained at 78° C. for four hours. The obtained reaction solution was reprecipitated twice in an excess amount of hexane and the precipitated resin was dried, whereby 96.5 g of a phenoxyethyl methacrylate/methyl methacrylate/methacrylic acid (copolymer ratio [mass ratio]=50/37/13) copolymer (water-insoluble resin P-1) was obtained.

후처리

  1. additionwas added dropwise
  2. waitAfter reacting for another hour
  3. additionafter the end of the dropwise addition
  4. additionwas added
  5. temperatureheated to and
  6. temperaturemaintained at 78° C. for four hours
  7. customThe obtained reaction solution
  8. customwas reprecipitated twice in an excess amount of hexane
  9. customthe precipitated resin was dried

출처 및 근거

ORD 기록
ord-1a5364f734454e22abd8b580cd685aea
출처 데이터셋
uspto-grants-2015_04
특허 번호
US09010916B2

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