반응 #1106654

ord-f4eea584a1434912b619602a0c84645e

반응 방정식

O=C1C=CC(=O)O1
Maleic Anhydride
CCCCC1CC2C=CC1C2
5-Butyl-2-norbornene
CC(C)(C#N)N=NC(C)(C)C#N
AIBN
CCCCC1CC2C=CC1C2.O=C1C=CC(=O)O1
MA BuNB
수율 78.0%

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 added to hexane (2 L)
  6. 6
    기타to give a white powder that
  7. 7
    여과was filtered
  8. 8
    기타dried in a vacuum oven at 80° C. for 1 hr

실험 절차

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).

출처

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