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Benzyl methacrylate → 1-Ethoxyethyl methacrylate (1-ethyl-3-oxacyclobutyl)methyl methacrylate benzyl methacrylate

HRID 2191188
ノート
印刷プレビュー

反応式

HRID 2191188 の反応式
[C:1]([O:6][CH:7]([O:9][CH2:10][CH3:11])[CH3:8])(=[O:5])[C:2]([CH3:4])=[CH2:3].[C:12]([O:17][CH2:18][C:19]1([CH2:23][CH3:24])[CH2:22][O:21][CH2:20]1)(=[O:16])[C:13]([CH3:15])=[CH2:14].[C:25]([O:30][CH2:31][C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1)(=[O:29])[C:26]([CH3:28])=[CH2:27].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][CH3:11])[CH3:8])(=[O:5])[C:2]([CH3:4])=[CH2:3].[C:12]([O:17][CH2:18][C:19]1([CH2:23][CH3:24])[CH2:20][O:21][CH2:22]1)(=[O:16])[C:13]([CH3:15])=[CH2:14].[C:25]([O:30][CH2:31][C:32]1[CH:33]=[CH:34][CH:35]=[CH:36][CH:37]=1)(=[O:29])[C:26]([CH3:28])=[CH2:27]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 17236Benzyl methacrylateHCID 11159706(3-Ethyloxetan-3-yl)methyl 2-methylprop-2-enoateHCID 201933451-Ethoxyethyl Methacrylate (stabilized with MEHQ)HCID 219175032,2'-Azobis(methyl 2-methylpropanate)

生成物 1

HCID 866432131-Ethoxyethyl methacrylate (1-ethyl-3-oxacyclobutyl)methyl methacrylate benzyl methacrylate

試薬・触媒・溶媒 2

HCID 7909Methyl Isobutyl Ketone溶媒
HCID 8900Heptane溶媒

実験手順

Into a 500 ml-volume three-neck flask, 47.5 g (0.3 mol) of 1-ethoxyethyl methacrylate, 33.2 g (0.18 mol) of (1-ethyl-3-oxacyclobutyl)methyl methacrylate, 21.2 g (0.12 mol) of benzyl methacrylate and 300 ml of methyl isobutyl ketone were charged. A catalytic amount of 2,2′-azobis(methyl 2-methylpropionate) was added thereto as a radical polymerization initiator, and polymerization was allowed to proceed at 80° C. for 6 hours in a nitrogen stream. The reaction solution was cooled and then poured in a large amount of heptane to precipitate a polymer. The crystal was collected by filtration and dissolved in diethylene glycol dimethyl ether, and heptane and methyl isobutyl ketone contained in the solution were removed by distillation under reduced pressure to obtain Polymer A-8 (1-ethoxyethyl methacrylate/(1-ethyl-3-oxacyclobutyl)methyl methacrylate/benzyl methacrylate) as a diethylene glycol dimethyl ether solution.

後処理

  1. customas a radical polymerization initiator, and polymerization
  2. temperatureThe reaction solution was cooled
  3. customto precipitate a polymer
  4. filtrationThe crystal was collected by filtration
  5. dissolutiondissolved in diethylene glycol dimethyl ether
  6. customwere removed by distillation under reduced pressure

出典と根拠

ORDレコード
ord-3fa215b08b0e429b8752dfa3a5329bab
出典データセット
uspto-grants-2012_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08329380B2

反応ノート

読み込み中…

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