2-Hydroxyethyl Methacrylate → 1-Cyclohexyloxyethyl methacrylate 3,4-epoxycyclohexylmethyl methacrylate 2-hydroxyethyl methacrylate

HRID 2191185

反応式

HRID 2191185 の反応式
[C:1]([O:6][CH:7]([O:9][CH:10]1[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]1)[CH3:8])(=[O:5])[C:2]([CH3:4])=[CH2:3].[C:16]([O:21][CH2:22][CH:23]1[CH2:28][CH2:27][CH:26]2[O:29][CH:25]2[CH2:24]1)(=[O:20])[C:17]([CH3:19])=[CH2:18].[C:30]([O:35][CH2:36][CH2:37][OH:38])(=[O:34])[C:31]([CH3:33])=[CH2:32].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][CH:10]1[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15]1)[CH3:8])(=[O:5])[C:2]([CH3:4])=[CH2:3].[C:16]([O:21][CH2:22][CH:23]1[CH2:28][CH2:27][CH:26]2[O:29][CH:25]2[CH2:24]1)(=[O:20])[C:17]([CH3:19])=[CH2:18].[C:30]([O:35][CH2:36][CH2:37][OH:38])(=[O:34])[C:31]([CH3:33])=[CH2:32]

参加物

7

反応物 4

HCID 133602-Hydroxyethyl MethacrylateHCID 14645478(7-Oxabicyclo(4.1.0)heptan-3-yl)methyl 2-methylprop-2-enoateHCID 219175032,2'-Azobis(methyl 2-methylpropanate)HCID 229952811-Cyclohexyloxyethyl methacrylate

生成物 1

HCID 866432101-Cyclohexyloxyethyl methacrylate 3,4-epoxycyclohexylmethyl methacrylate 2-hydroxyethyl 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, 76.4 g (0.36 mol) of 1-cyclohexyloxyethyl methacrylate, 35.3 g (0.18 mol) of 3,4-epoxycyclohexylmethyl methacrylate (Cyclomer M100, produced by Daicel Chemical Industries, Ltd.), 7.8 g (0.06 mol) of 2-hydroxyethyl 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-5 (1-cyclohexyloxyethyl methacrylate/3,4-epoxycyclohexylmethyl methacrylate/2-hydroxyethyl 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-effc43291b5a4d58bf5cfcb7ee348b26
出典データセット
uspto-grants-2012_12
特許番号
US08329380B2

関連ノート

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