反応 #1106655

反応方程式

Maleic Anhydride

2-Norbornene

5-Butyl-2-norbornene

AIBN

→

MA NB BuNB

収率 112.9%

溶媒

THF

反応条件

後処理

1. 1
   workup.ADDITIONcharged to an appropriately sized reaction vessel
2. 2
   その他The solution was sparged with nitrogen for 10 min
3. 3
   その他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
   その他to give a white powder that
8. 8
   ろ過was filtered
9. 9
   その他dried in a vacuum oven at 80° C. for 16 hr

実験手順

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).

出典