反応 #1106653

ord-73cee0248ebe481396b5548784831e09

反応方程式

O=C1C=CC(=O)O1
Maleic Anhydride
C1=CC2CCC1C2
2-Norbornene
CC(C)(C#N)N=NC(C)(C)C#N
AIBN
C1=CC2CCC1C2.O=C1C=CC(=O)O1
MA NB
収率 90.2%

溶媒

反応条件

温度
70°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONcharged to an appropriately sized reaction vessel
  2. 2
    その他The solution was sparged with nitrogen for 10 min
  3. 3
    その他to remove oxygen
  4. 4
    温度after which the solution was cooled to room temperature
  5. 5
    workup.ADDITIONThe reaction mixture was then diluted with 2.0 g of THF
  6. 6
    workup.ADDITIONwas added to hexane (1 L)
  7. 7
    その他to give a white powder that
  8. 8
    ろ過was filtered
  9. 9
    その他dried in a vacuum oven at 80° C. for 16 hr

実験手順

Maleic Anhydride (MA, 7.4 g, 75.0 mmol), 2-Norbornene (NB, 7.1 g, 75.0 mmol) and AIBN (1.2 g, 7.5 mmol) was dissolved in THF (20.4 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 5.0 hr, after which the solution was cooled to room temperature. The reaction mixture was then diluted with 2.0 g of THF and was 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, 13.0 g (90%) of the MA/NB polymer was isolated (GPC Mw=4,100 Mn=1,800).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08715900B2uspto-grants-2014_05