Reaktion #1106654

ord-f4eea584a1434912b619602a0c84645e

Reaktionsgleichung

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
Ausbeute 78.0%

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

Vorschrift

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).

Quelle

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