Reaktion #9611

Reaktionsgleichung

benzoyl peroxide

benzoyl peroxide

n-octylphosphinic acid

1-octene

benzoyl peroxide

→

di-n-octylphosphinic acid

Ausbeute 48.4%

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONwas added
2. 2
   TemperaturThe resulting mixture was refluxed for 8 hs
3. 3
   Temperaturto reflux for an extra 8 hs
4. 4
   Temperaturrefluxing
5. 5
   TemperaturThe resulting mixture was cooled in the refrigerator
6. 6
   Filtrationfiltered
7. 7
   Sonstige11.8 g of di-n-octylphosphinic acid was recovered
8. 8
   Sonstigea rotary evaporator
9. 9
   WaschenThe solid was washed with 100 mL of cooled 95% ethanol
10. 10
    Einengenthe filtrate was concentrated on the rotary vacuum

Vorschrift

To a stirred mixture of 46.5 g (0.261 mol) of n-octylphosphinic acid in 250 mL 95% ethanol, 1-octene (58.6 g, 0.5218 mol) was added followed by 9.042 g (0.026 mol) of 70% benzoyl peroxide. The resulting mixture was refluxed for 8 hs, and then another 6.758 g (0.0196 mol) of benzoyl peroxide was added and the reaction continued to reflux for an extra 8 hs. A third 4.244 g of benzoyl peroxide was added (0.01305 mol) and refluxing continued for an extra 8 hs. The resulting mixture was cooled in the refrigerator, filtered, and 11.8 g of di-n-octylphosphinic acid was recovered using a rotary evaporator. The solid was washed with 100 mL of cooled 95% ethanol and the filtrate was concentrated on the rotary vacuum and replaced in the refrigerator. Another 24.9 g di-n-octylphosphinic acid was obtained on cooling to attain a total of 36.7 g (48.4% yield).

Quelle