Azobisisobutyronitrile → MA BuNB

HRID 1019472

反応式

HRID 1019472 の反応式
[C:1]1(=[O:7])[O:6][C:4](=[O:5])[CH:3]=[CH:2]1.[CH2:8]([CH:12]1[CH2:17][CH:16]2[CH2:18][CH:13]1[CH:14]=[CH:15]2)[CH2:9][CH2:10][CH3:11].CC(N=NC(C#N)(C)C)(C#N)C>C1COCC1>[C:4]1(=[O:5])[O:6][C:1](=[O:7])[CH:2]=[CH:3]1.[CH2:8]([CH:12]1[CH2:17][CH:16]2[CH2:18][CH:13]1[CH:14]=[CH:15]2)[CH2:9][CH2:10][CH3:11]

参加物

5

反応物 3

HCID 6547AzobisisobutyronitrileHCID 7923Maleic AnhydrideHCID 168020Bicyclo[2.2.1]hept-2-ene, 5-butyl-

生成物 1

HCID 131731366MA BuNB収率 78%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
70 °C

実験手順

Maleic Anhydride (MA, 9.8 g, 100 mmol), 5-Butyl-2-norbornene (BuNB, 15.0 g, 100 mmol) and AIBN (1.64 g, 10.0 mmol) was dissolved in THF (37.2 g) and charged to an appropriately sized reaction vessel. The solution was sparged with nitrogen for 10 min to remove oxygen and then heated to 70 ° C. The mixture was allowed to stir at 70° C. for 16 hr, after which the solution was cooled to room temperature. The reaction mixture was added to hexane (2 L) to give a white powder that was filtered and dried in a vacuum oven at 80° C. for 1 hr. Approximately, 19.3 g (78%) of the MA/BuNB polymer was isolated (GPC Mw=3,200 Mn=1,900).

後処理

  1. additioncharged to an appropriately sized reaction vessel
  2. customThe solution was sparged with nitrogen for 10 min
  3. customto remove oxygen
  4. temperatureafter which the solution was cooled to room temperature
  5. additionThe reaction mixture was added to hexane (2 L)
  6. customto give a white powder that
  7. filtrationwas filtered
  8. customdried in a vacuum oven at 80° C. for 1 hr

出典と根拠

ORDレコード
ord-f4eea584a1434912b619602a0c84645e
出典データセット
uspto-grants-2014_05
特許番号
US08715900B2

関連ノート

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