反応 #1382969

反応方程式

di-(n-decyl)cyclopentadiene

1,10-decanediol

KOH

triglyme

→

Di-(n-decyl)cyclopentane

反応条件

後処理

1. 1
   その他In a one-liter three-necked flask fitted with a mechanical stirrer
2. 2
   その他topped with a condenser
3. 3
   その他deoxygenated with a stream of nitrogen
4. 4
   温度The mixture was then heated
5. 5
   温度to reflux under nitrogen for two hours
6. 6
   温度The mixture was cooled
7. 7
   洗浄washed with water
8. 8
   その他to remove base and triglyme
9. 9
   その他The product was dried
10. 10
    workup.ADDITIONcontaining a higher number of crosslinked di(n-decyl)cyclopentadienes
11. 11
    その他were formed
12. 12
    その他at 100°

実験手順

In a one-liter three-necked flask fitted with a mechanical stirrer and a Soxhlet extractor packed with 3A molecular sieves (about 15 g) and topped with a condenser, 25.1 g of di-(n-decyl)cyclopentadiene (73 mmol), 12.6 g of 1,10-decanediol (73 mmol), 5 g of KOH, and 250 g of triglyme were stirred and deoxygenated with a stream of nitrogen. The mixture was then heated to reflux under nitrogen for two hours. The mixture was cooled and washed with water to remove base and triglyme. The product was dried and hydrogenated over palladium on carbon. The resulting product was characterized by gel permeation chromatography to determine the molecular weight. The number average molecular weight was 1250, indicating that on average about 3 di(n-decyl)cyclopentadienes had been crosslinked. The weight average molecular weight of 2250 indicates that molecules containing a higher number of crosslinked di(n-decyl)cyclopentadienes were formed. The measured viscosity at 100°, 40 cSt, is consistent with these high molecular weights.

出典