반응 #1106653

ord-73cee0248ebe481396b5548784831e09

반응 방정식

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
수율 90.2%

용매

반응 조건

온도
70°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONcharged to an appropriately sized reaction vessel
  2. 2
    기타The solution was sparged with nitrogen for 10 min
  3. 3
    기타to remove oxygen
  4. 4
    온도after 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
    기타to give a white powder that
  8. 8
    여과was filtered
  9. 9
    기타dried in a vacuum oven at 80° C. for 16 hr

실험 절차

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).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08715900B2uspto-grants-2014_05