反应 #1106654

ord-f4eea584a1434912b619602a0c84645e

反应方程式

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
收率 78.0%

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 added to hexane (2 L)
  6. 6
    其他to give a white powder that
  7. 7
    过滤was filtered
  8. 8
    其他dried in a vacuum oven at 80° C. for 1 hr

实验过程

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).

来源

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