反応 #661206

ord-0f00b9825d854a42998bbc8a14935fbe

反応方程式

C=C(C)C(=O)OC1CCCCO1
2-tetrahydropyranyl methacrylate
C=Cc1ccc(OC(C)=O)cc1
p-acetoxystyrene
C=C(C)C(=O)OCCO
2-hydroxyethyl methacrylate
CCC(C)(N=NC(C)(CC)C(=O)[O-])C(=O)[O-]
2,2′-azobis(methyl 2-methylpropionate)
CCOCCOCCOC
diethylene glycol ethyl methyl ether
C=C(C)C(=O)OC1CCCCO1.C=C(C)C(=O)OCCO.C=Cc1ccc(OC(C)=O)cc1
2-tetrahydropyranyl methacrylate p-acetoxystyrene 2-hydroxyethyl methacrylate
COCC(C)OC(C)=O
propylene glycol monomethyl ether acetate

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他as a radical polymerization initiator, and polymerization
  2. 2
    温度The reaction solution was cooled
  3. 3
    その他to precipitate a polymer
  4. 4
    ろ過The crystal was collected by filtration
  5. 5
    workup.DISSOLUTIONdissolved in a mixed solvent of propylene glycol monomethyl ether acetate and diethylene glycol ethyl methyl ether, and heptane and methyl isobutyl ketone
  6. 6
    その他were removed by distillation under reduced pressure

実験手順

Into a 500 ml-volume three-neck flask, 71.5 g (0.42 mol) of 2-tetrahydropyranyl methacrylate, 19.5 g (0.12 mol) of p-acetoxystyrene, 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 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 A1-7 (2-tetrahydropyranyl methacrylate/p-acetoxystyrene/2-hydroxyethyl methacrylate) as a solution in a mixed solvent of propylene glycol monomethyl ether acetate and diethylene glycol ethyl methyl ether.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09034440B2uspto-grants-2015_05