tert-Butyl methacrylate → 4-Acetoxystyrene tert-butyl methacrylate (4-phenyl)phenyl methacrylate

HRID 44122

反応式

HRID 44122 の反応式
[C:1]([O:4][C:5]1[CH:12]=[CH:11][C:8]([CH:9]=[CH2:10])=[CH:7][CH:6]=1)(=[O:3])[CH3:2].[C:13]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])(=[O:17])[C:14]([CH3:16])=[CH2:15].[C:23]([O:28][C:29]1[CH:34]=[CH:33][C:32]([C:35]2[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=2)=[CH:31][CH:30]=1)(=[O:27])[C:24]([CH3:26])=[CH2:25].N(C(C)(C)C(OC)=O)=NC(C)(C)C(OC)=O>C1(=O)CCCCC1.CCCCCC>[C:1]([O:4][C:5]1[CH:12]=[CH:11][C:8]([CH:9]=[CH2:10])=[CH:7][CH:6]=1)(=[O:3])[CH3:2].[C:13]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])(=[O:17])[C:14]([CH3:16])=[CH2:15].[C:23]([O:28][C:29]1[CH:34]=[CH:33][C:32]([C:35]2[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=2)=[CH:31][CH:30]=1)(=[O:27])[C:24]([CH3:26])=[CH2:25]

参加物

7

反応物 4

HCID 11448tert-Butyl methacrylateHCID 757631,1'-Dimethyl 2,2'-(1,2-diazenediyl)bis(2-methylpropanoate)HCID 758214-Ethenylphenyl acetateHCID 112878602-Methyl-acrylic acid biphenyl-4-YL ester

生成物 1

HCID 866607604-Acetoxystyrene tert-butyl methacrylate (4-phenyl)phenyl methacrylate収率 873.9%

試薬・触媒・溶媒 2

HCID 7967Cyclohexanone溶媒2 回HCID 8058Hexane溶媒

実験手順

31.63 Gram (0.195 mol) of 4-acetoxystyrene, 13.65 g (0.096 mol) of tert-butyl methacrylate, 2.14 g (0.009 mol) of (4-phenyl)phenyl methacrylate and 3.45 g (0.015 mol) of polymerization initiator V-601 (produced by Wako Pure Chemical Industries, Ltd.) were dissolved in 151.75 g of cyclohexanone. Subsequently, 37.94 g of cyclohexanone was charged into a reaction vessel, and the solution above was added dropwise to the system at 80° C. over 6 hours in a nitrogen gas atmosphere. After the completion of dropwise addition, the reaction solution was stirred for 2 hours, then allowed to cool to room temperature and added dropwise in 2.5 L of hexane to precipitate a polymer, followed by filtration. The solid collected by filtration was washed by splashing 500 mL of hexane thereon and then dried under reduced pressure to obtain 42.68 g of a 4-acetoxystyrene/tert-butyl methacrylate/(4-phenyl)phenyl methacrylate copolymer.

後処理

  1. additionthe solution above was added dropwise to the system at 80° C. over 6 hours in a nitrogen gas atmosphere
  2. additionAfter the completion of dropwise addition
  3. customto precipitate a polymer
  4. filtrationfollowed by filtration
  5. filtrationThe solid collected by filtration
  6. washwas washed
  7. customdried under reduced pressure

出典と根拠

ORDレコード
ord-544c610998c946a78a2d3f67339e30a4
出典データセット
uspto-grants-2013_09
特許番号
US08541161B2

関連ノート

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