Methacrylic Acid → 3,4-Epoxycyclohexylmethyl methacrylate benzyl methacrylate methacrylic acid

HRID 574027노트

반응식

HRID 574027 반응식
[C:1]([O:6][CH2:7][CH:8]1[CH2:13][CH2:12][CH:11]2[O:14][CH:10]2[CH2:9]1)(=[O:5])[C:2]([CH3:4])=[CH2:3].[C:15]([O:20][CH2:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)(=[O:19])[C:16]([CH3:18])=[CH2:17].[C:28]([OH:33])(=[O:32])[C:29]([CH3:31])=[CH2:30].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][CH2:7][CH:8]1[CH2:13][CH2:12][CH:11]2[O:14][CH:10]2[CH2:9]1)(=[O:5])[C:2]([CH3:4])=[CH2:3].[C:15]([O:20][CH2:21][C:22]1[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=1)(=[O:19])[C:16]([CH3:18])=[CH2:17].[C:28]([OH:33])(=[O:32])[C:29]([CH3:31])=[CH2:30]

참가 물질

7

반응물 4

HCID 4093Methacrylic AcidHCID 17236Benzyl methacrylateHCID 14645478(7-Oxabicyclo(4.1.0)heptan-3-yl)methyl 2-methylprop-2-enoateHCID 219175032,2'-Azobis(methyl 2-methylpropanate)

생성물 1

HCID 866555463,4-Epoxycyclohexylmethyl methacrylate benzyl methacrylate methacrylic acid

시약·촉매·용매 2

HCID 7909Methyl Isobutyl Ketone용매HCID 8900Heptane용매

실험 절차

Into a 500 ml-volume three-neck flask, 58.9 g (0.30 mol) of 3,4-epoxycyclohexylmethyl methacrylate (Cyclomer M100, produced by Daicel Chemical Industries, Ltd.), 31.7 g (0.18 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 diethylene glycol dimethyl ether, and heptane and methyl isobutyl ketone contained in the solution were removed by distillation under reduced pressure to obtain Polymer A2-3 (3,4-epoxycyclohexylmethyl methacrylate/benzyl methacrylate/methacrylic acid) as a diethylene glycol dimethyl ether solution.

후처리

  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

출처 및 근거

ORD 기록
ord-f0b569f1ff9d4984a01f8dd1979814df
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09034440B2

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