Reacción #1106653

ord-73cee0248ebe481396b5548784831e09

Ecuación de reacción

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
Rendimiento 90.2%

Reactivos

Ninguno

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 then diluted with 2.0 g of THF
  6. 6
    workup.ADDITIONwas added to hexane (1 L)
  7. 7
    Otroto give a white powder that
  8. 8
    Filtraciónwas filtered
  9. 9
    Otrodried in a vacuum oven at 80° C. for 16 hr

Procedimiento

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).

Fuente

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