反应 #1106655

ord-3b233f6626ca48a4ad2981d1e47337d0

反应方程式

O=C1C=CC(=O)O1
Maleic Anhydride
C1=CC2CCC1C2
2-Norbornene
CCCCC1CC2C=CC1C2
5-Butyl-2-norbornene
CC(C)(C#N)N=NC(C)(C)C#N
AIBN
C1=CC2CCC1C2.CCCCC1CC2C=CC1C2.O=C1C=CC(=O)O1
MA NB BuNB
收率 112.9%

溶剂

反应条件

温度
70°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.ADDITIONcharged to an appropriately sized reaction vessel
  2. 2
    其他The solution was sparged with nitrogen for 10 min
  3. 3
    其他to remove oxygen
  4. 4
    温度after which the solution was cooled to room temperature
  5. 5
    workup.ADDITIONThe reaction mixture was diluted with 20 g of THF
  6. 6
    workup.ADDITIONadded to hexane (1 L)
  7. 7
    其他to give a white powder that
  8. 8
    过滤was filtered
  9. 9
    其他dried in a vacuum oven at 80° C. for 16 hr

实验过程

Maleic Anhydride (MA, 7.4 g, 75.0 mmol), 2-Norbornene (NB, 3.5 g, 37.5 mmol), 5-Butyl-2-norbornene (BuNB, 5.6 g, 37.5 mmol) and AIBN (1.2 g, 7.5 mmol) was dissolved in THF (23.6 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 20.5 hr, after which the solution was cooled to room temperature. The reaction mixture was diluted with 20 g of THF and 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, 14.5 g (88%) of the MA/NB/BuNB polymer was isolated (GPC Mw=3,500 Mn=1,700).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08715900B2uspto-grants-2014_05