Methacrylic Acid → Propylene glycol methyl ether acetate

HRID 574018ノート

反応式

HRID 574018 の反応式
[C:1]([O:6][CH:7]([O:9][CH2:10][CH2:11][CH2:12][CH3:13])[CH3:8])(=[O:5])[C:2]([CH3:4])=[CH2:3].[C:14]([O:19][CH2:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)(=[O:18])[C:15]([CH3:17])=[CH2:16].[C:27]([OH:32])(=[O:31])[C:28]([CH3:30])=[CH2:29].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][CH2:11][CH2:12][CH3:13])[CH3:8])(=[O:5])[C:2]([CH3:4])=[CH2:3].[C:14]([O:19][CH2:20][C:21]1[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=1)(=[O:18])[C:15]([CH3:17])=[CH2:16].[C:27]([OH:32])(=[O:31])[C:28]([CH3:30])=[CH2:29].[C:7]([O:9][CH:10]([CH3:11])[CH2:14][O:19][CH3:20])(=[O:6])[CH3:8]

参加物

8

反応物 4

HCID 4093Methacrylic AcidHCID 17236Benzyl methacrylateHCID 219175032,2'-Azobis(methyl 2-methylpropanate)HCID 219599501-Butoxyethyl methacrylate

生成物 2

HCID 7946Propylene glycol methyl ether acetateHCID 866555401-n-Butoxyethyl methacrylate benzyl methacrylate methacrylic acid

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, 67.1 g (0.36 mol) of 1-n-butoxyethyl methacrylate, 21.1 g (0.12 mol) of benzyl methacrylate, 10.3 g (0.12 mol) of methacrylic acid 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 propylene glycol monomethyl ether acetate, and heptane and methyl isobutyl ketone contained in the solution were removed by distillation under reduced pressure to obtain Polymer A1-1 (1-n-butoxyethyl methacrylate/benzyl methacrylate/methacrylic acid) as a propylene glycol monomethyl ether acetate 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 propylene glycol monomethyl ether acetate
  6. customwere removed by distillation under reduced pressure

出典と根拠

ORDレコード
ord-927f755dd5ed416994ce6d6f5ec25027
出典データセット
uspto-grants-2015_05
特許番号
US09034440B2

反応ノート

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