Oxygen → Isobutene Isobornyl Acrylate

HRID 1264143

反応式

HRID 1264143 の反応式
[CH3:1][C@@:2]12[CH:10]([C:11]([C:13]([O-:15])=[O:14])=[CH2:12])[CH2:9][C@H:5]([C:6]1([CH3:8])[CH3:7])[CH2:4][CH2:3]2.CCCCC(C1C=CN=C(C2C=C(C(CCCC)CCCC)C=CN=2)C=1)CCCC.O=O>>[CH2:1]=[C:2]([CH3:6])[CH3:3].[CH3:1][C@@:2]12[CH:10]([C:11]([C:13]([O-:15])=[O:14])=[CH2:12])[CH2:9][C@H:5]([C:6]1([CH3:7])[CH3:8])[CH2:4][CH2:3]2

参加物

4

反応物 3

HCID 977OxygenHCID 1749844,4'-Bis(1-butylpentyl)-2,2'-bipyridineHCID 92004758Isobomyl acrylate3 回

生成物 1

HCID 131723834Isobutene Isobornyl Acrylate

反応条件

温度
0 °C

実験手順

The following reagents were weighed into a glass tube under ambient temperature: 0.3 g(3×10−7 mol) brominated p-methylstyrene-isobutene elastomer (Exxon) (Mn=108380, Mw/Mn=2.31), 12 mg (8.37×10−2 mmol) of CuBr, 1.00 mL (0.986 g, 5 mmol) of isobornyl acrylate, and 60 mg (0.175 mmol) 4,4′-di-(5-nonyl)-2,2′-bipyridine. Two “freeze-pump-thaw” cycles were performed on the contents of the tube to insure that oxygen was removed from the polymerization solution. The tube was sealed under vacuum and placed in an oil bath thermostated at 90 C. After 2 h the tube was removed from the oil bath and cooled to 0° C. to quench the polymerization. Conversion of the monomer was measured using GC; the molecular weight and polydispersity were measured by GPC. Conversion of isobornyl acrylate was 30%, Mn=141000, Mw/Mn=2.61. 1H NMR spectrum showed that the graft copolymer contained 30% isobornyl acrylate. By DSC measurement one Tg was found at 2° C.

後処理

  1. customThe following reagents were weighed into a glass tube under ambient temperature
  2. customwas removed from the polymerization solution
  3. customThe tube was sealed under vacuum
  4. customplaced in an oil bath
  5. customAfter 2 h the tube was removed from the oil bath
  6. customto quench
  7. customthe polymerization
  8. customwas found at 2° C.

出典と根拠

ORDレコード
ord-98f2a43f81434cc98a32c293427376a6
出典データセット
uspto-grants-2003_04
特許番号
US06541580B1

関連ノート

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