Reacción #1106654

ord-f4eea584a1434912b619602a0c84645e

Ecuación de reacción

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
Rendimiento 78.0%

Disolventes

Condiciones de reacción

Temperatura
70°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    workup.ADDITIONcharged to an appropriately sized reaction vessel
  2. 2
    OtroThe solution was sparged with nitrogen for 10 min
  3. 3
    Otroto remove oxygen
  4. 4
    Temperaturaafter which the solution was cooled to room temperature
  5. 5
    workup.ADDITIONThe reaction mixture was added to hexane (2 L)
  6. 6
    Otroto give a white powder that
  7. 7
    Filtraciónwas filtered
  8. 8
    Otrodried in a vacuum oven at 80° C. for 1 hr

Procedimiento

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).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08715900B2uspto-grants-2014_05