Reaktion #1106653

ord-73cee0248ebe481396b5548784831e09

Reaktionsgleichung

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
Ausbeute 90.2%

Lösungsmittel

Reaktionsbedingungen

Temperatur
70°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

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

Vorschrift

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).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08715900B2uspto-grants-2014_05