Methacrylic Acid → 1-Benzyloxyethyl methacrylate 2-hydroxyethyl methacrylate methacrylic acid

HRID 1618832ノート

反応式

HRID 1618832 の反応式
[C:1]([O:6][CH:7]([O:9][CH2:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)[CH3:8])(=[O:5])[C:2]([CH3:4])=[CH2:3].[C:17]([O:22][CH2:23][CH2:24][OH:25])(=[O:21])[C:18]([CH3:20])=[CH2:19].[C:26]([OH:31])(=[O:30])[C:27]([CH3:29])=[CH2:28].N(C(C)(CC)C([O-])=O)=NC(C)(CC)C([O-])=O>CCCCCCC.C(C(C)=O)C(C)C>[C:1]([O:6][CH:7]([O:9][CH2:10][C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=1)[CH3:8])(=[O:5])[C:2]([CH3:4])=[CH2:3].[C:17]([O:22][CH2:23][CH2:24][OH:25])(=[O:21])[C:18]([CH3:20])=[CH2:19].[C:26]([OH:31])(=[O:30])[C:27]([CH3:29])=[CH2:28]

参加物

7

反応物 4

HCID 4093Methacrylic AcidHCID 133602-Hydroxyethyl MethacrylateHCID 218349871-Benzyloxyethyl methacrylateHCID 219175032,2'-Azobis(methyl 2-methylpropanate)

生成物 1

HCID 866555411-Benzyloxyethyl methacrylate 2-hydroxyethyl methacrylate methacrylic acid

試薬・触媒・溶媒 2

HCID 7909Methyl Isobutyl Ketone溶媒HCID 8900Heptane溶媒

実験手順

A 500 ml three-necked flask was charged with 105.7 g (0.48 mol) of 1-benzyloxyethyl methacrylate, 7.8 g (0.06 mol) of 2-hydroxyethyl methacrylate, 5.2 g (0.06 mol) of methacrylic acid and 300 ml of methyl isobutyl ketone. A catalytic amount of 2,2′-azobis(methyl 2-methylpropionate) as a radical polymerization initiator was added to the mixture, and polymerization was performed in a nitrogen stream at 80° C. for six hours. The obtained reaction liquid was cooled, and poured in a large volume of heptane, thereby precipitating a polymer. The polymer crystal was collected by filtration, and dissolved in diethylene glycol dimethyl ether. The heptane and methyl isobutyl ketone contained in the solution were distilled off in vacuum, thereby obtaining a diethylene glycol dimethyl ether solution of polymer A1-2 (1-benzyloxyethyl methacrylate/2-hydroxyethyl methacrylate/methacrylic acid).

後処理

  1. customThe obtained reaction liquid
  2. temperaturewas cooled
  3. customprecipitating a polymer
  4. filtrationThe polymer crystal was collected by filtration
  5. dissolutiondissolved in diethylene glycol dimethyl ether
  6. distillationwere distilled off in vacuum

出典と根拠

ORDレコード
ord-59b0283b764642e0aaec2b3c29fbe1c8
出典データセット
uspto-grants-2014_07
特許番号
US08771907B2

反応ノート

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