反应 #1106656

ord-7d910bea30ed47aaa3f79b2c6d925c26

反应方程式

O=C1C=CC(=O)O1
Maleic Anhydride
CCC12CCC(C=C1c1ccccc1)C2
Phenyl Ethyl Norbornene
CC(C)(C#N)N=NC(C)(C)C#N
AIBN
CCC12CCC(C=C1c1ccccc1)C2.O=C1C=CC(=O)O1
MA PENB
收率 75.1%

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 30 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), Phenyl Ethyl Norbornene (PENB, 14.9 g, 75.0 mmol) and AIBN (1.2 g, 7.5 mmol) was dissolved in THF (32.1 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 17.5 hr, after which the solution was cooled to room temperature. The reaction mixture was diluted with 30 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, 16.7 g (75%) of the MA/PENB polymer was isolated (GPC Mw=3,400 Mn=1,500).

来源

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