Azobisisobutyronitrile → ZINC methacrylate ethylene glycol dimethacrylate

HRID 1167034

反応式

HRID 1167034 の反応式
[C:1]([O-:6])(=[O:5])[C:2]([CH3:4])=[CH2:3].[Zn+2:7].[C:8]([O-:13])(=[O:12])[C:9]([CH3:11])=[CH2:10].[C:14]([O:19][CH2:20][CH2:21][O:22][C:23](=[O:27])[C:24]([CH3:26])=[CH2:25])(=[O:18])[C:15]([CH3:17])=[CH2:16].CC(N=NC(C#N)(C)C)(C#N)C.N(C1(C#N)CCCCC1)=NC1(C#N)CCCCC1>CN(C)C=O>[C:1]([O-:6])(=[O:5])[C:2]([CH3:4])=[CH2:3].[Zn+2:7].[C:8]([O-:13])(=[O:12])[C:9]([CH3:11])=[CH2:10].[C:14]([O:19][CH2:20][CH2:21][O:22][C:23](=[O:27])[C:24]([CH3:26])=[CH2:25])(=[O:18])[C:15]([CH3:17])=[CH2:16]

参加物

6

反応物 4

HCID 6547AzobisisobutyronitrileHCID 7355Ethylene glycol dimethacrylateHCID 749781,1'-Azobis(cyclohexanecarbonitrile)HCID 101308962-Propenoic acid, 2-methyl-, zinc salt (2:1)

生成物 1

HCID 131724062ZINC methacrylate ethylene glycol dimethacrylate

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Zinc methacrylate (848 mg, 3.6 mmol), ethylene glycol dimethacrylate (678 ml, 3.6 mmol) and the radical initiator VAZO® (1,1′-azobis(cyclohexanecarbonitrile), Aldrich) (20 mg, 0.08 mmol) were dissolved in dimethylformamide (15 ml) in a borosilicate test tube. The solution was sonicated for 1 min and sparged with nitrogen. The test tube was covered with parafilm. The reaction mixture was stirred and placed in an oil bath which was then heated slowly over 1.5 hrs to 95° C. When the reaction mixture reached a temperature of 85° C., a precipitate started to form. Heating was continued for a total of 6 hrs and the polymer was left at room temperature overnight. The white polymer particles were filtered off and extracted with methanol in a Soxhlet apparatus for 8 hrs. The fines were removed by suspending particles in water and discarding the supernatant. This step was repeated until the supernatant was clear. The remaining polymer was filtered off and rinsed with methanol. The polymer was left to dry for 2 hours at room temperature, followed by overnight drying at 140° C.

後処理

  1. customThe solution was sonicated for 1 min
  2. customsparged with nitrogen
  3. customplaced in an oil bath
  4. temperaturewhich was then heated slowly over 1.5 hrs to 95° C
  5. customa temperature of 85° C.
  6. customto form
  7. temperatureHeating
  8. customwas continued for a total of 6 hrs
  9. filtrationThe white polymer particles were filtered off
  10. extractionextracted with methanol in a Soxhlet apparatus for 8 hrs
  11. customThe fines were removed
  12. filtrationThe remaining polymer was filtered off
  13. washrinsed with methanol
  14. waitThe polymer was left
  15. customto dry for 2 hours at room temperature
  16. waitfollowed by overnight
  17. customdrying at 140° C.

出典と根拠

ORDレコード
ord-bb665a4d587f4fbeac48e19ad5a9fadb
出典データセット
uspto-grants-2003_09
特許番号
US06616846B2

関連ノート

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