Methacrylic Acid → Propylene glycol methyl ether acetate

HRID 1425627

反応式

HRID 1425627 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][CH:19]1[O:21][CH2:20]1)(=[O:16])[C:13]([CH3:15])=[CH2:14].[C:22]([O:27][CH2:28][C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1)(=[O:26])[C:23]([CH3:25])=[CH2:24].[C:35]([OH:40])(=[O:39])[C:36]([CH3:38])=[CH2:37].N([C:50](C)(CC)[C:51]([O-:53])=O)=N[C:43](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][CH:19]1[O:21][CH2:20]1)(=[O:16])[C:13]([CH3:15])=[CH2:14].[C:22]([O:27][CH2:28][C:29]1[CH:30]=[CH:31][CH:32]=[CH:33][CH:34]=1)(=[O:26])[C:23]([CH3:25])=[CH2:24].[C:35]([OH:40])(=[O:39])[C:36]([CH3:38])=[CH2:37].[C:12]([O:17][CH:18]([CH3:43])[CH2:19][O:21][CH3:20])(=[O:16])[CH3:13].[CH3:20][O:21][CH2:19][CH2:18][O:17][CH2:12][CH2:13][O:53][CH2:51][CH3:50]

参加物

10

反応物 5

HCID 4093Methacrylic AcidHCID 7837Glycidyl methacrylateHCID 17236Benzyl methacrylateHCID 201933451-Ethoxyethyl Methacrylate (stabilized with MEHQ)HCID 219175032,2'-Azobis(methyl 2-methylpropanate)

生成物 3

HCID 7946Propylene glycol methyl ether acetateHCID 138471-Ethoxy-2-(2-methoxyethoxy)ethaneHCID 866432121-Ethoxyethyl methacrylate glycidyl 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, 38.0 g (0.24 mol) of 1-ethoxyethyl methacrylate, 21.3 g (0.15 mol) of glycidyl methacrylate, 26.4 g (0.15 mol) of benzyl methacrylate, 5.2 g (0.06 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 a mixed solvent of propylene glycol monomethyl ether acetate and diethylene glycol ethyl methyl ether, and heptane and methyl isobutyl ketone contained in the solution were removed by distillation under reduced pressure to obtain Polymer A-7 (1-ethoxyethyl methacrylate/glycidyl methacrylate/benzyl methacrylate/methacrylic acid) as a solution in a mixed solvent of propylene glycol monomethyl ether acetate and diethylene glycol ethyl methyl ether.

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 a mixed solvent of propylene glycol monomethyl ether acetate and diethylene glycol ethyl methyl ether, and heptane and methyl isobutyl ketone
  6. customwere removed by distillation under reduced pressure

出典と根拠

ORDレコード
ord-5f408d51f6004fbe98eac9ff6ee70eff
出典データセット
uspto-grants-2015_01
特許番号
US08932800B2

関連ノート

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