Реакция #1106654

ord-f4eea584a1434912b619602a0c84645e

Уравнение реакции

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
Выход 78.0%

Реагенты

Нет

Растворители

Условия реакции

Температура
70°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

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

Методика

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).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08715900B2uspto-grants-2014_05