Azobisisobutyronitrile → MA NB BuNB

HRID 1019473ノート

反応式

HRID 1019473 の反応式
[C:1]1(=[O:7])[O:6][C:4](=[O:5])[CH:3]=[CH:2]1.[CH:8]12[CH2:14][CH:11]([CH2:12][CH2:13]1)[CH:10]=[CH:9]2.[CH2:15]([CH:19]1[CH2:24][CH:23]2[CH2:25][CH:20]1[CH:21]=[CH:22]2)[CH2:16][CH2:17][CH3:18].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.[CH:8]12[CH2:14][CH:11]([CH2:12][CH2:13]1)[CH:10]=[CH:9]2.[CH2:15]([CH:19]1[CH2:24][CH:23]2[CH2:25][CH:20]1[CH:21]=[CH:22]2)[CH2:16][CH2:17][CH3:18]

参加物

6

反応物 4

HCID 6547AzobisisobutyronitrileHCID 7923Maleic AnhydrideHCID 103522-NorborneneHCID 168020Bicyclo[2.2.1]hept-2-ene, 5-butyl-

生成物 1

HCID 131731367MA NB BuNB収率 112.9%

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, 7.4 g, 75.0 mmol), 2-Norbornene (NB, 3.5 g, 37.5 mmol), 5-Butyl-2-norbornene (BuNB, 5.6 g, 37.5 mmol) and AIBN (1.2 g, 7.5 mmol) was dissolved in THF (23.6 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 20.5 hr, after which the solution was cooled to room temperature. The reaction mixture was diluted with 20 g of THF and added to hexane (1 L) to give a white powder that was filtered and dried in a vacuum oven at 80° C. for 16 hr. Approximately, 14.5 g (88%) of the MA/NB/BuNB polymer was isolated (GPC Mw=3,500 Mn=1,700).

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 diluted with 20 g of THF
  6. additionadded to hexane (1 L)
  7. customto give a white powder that
  8. filtrationwas filtered
  9. customdried in a vacuum oven at 80° C. for 16 hr

出典と根拠

ORDレコード
ord-3b233f6626ca48a4ad2981d1e47337d0
出典データセット
uspto-grants-2014_05
特許番号
US08715900B2

反応ノート

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