Hydrochloric Acid → Trioctylphosphine oxide

HRID 1580330

Reaktionsgleichung

Reaktionsgleichung von HRID 1580330
[CH2:1](Cl)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8].[Mg].[P:11](Cl)(Cl)(Cl)=[O:12].Cl>C1(C)C(C)=CC=CC=1.O.C(OCC)C>[CH2:1]([P:11](=[O:12])([CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8])[CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8]

Komponenten

8

Edukt 4

HCID 313Hydrochloric AcidHCID 81421-Chlorooctane3×HCID 24813Phosphorus oxychlorideHCID 5462224Magnesium

Produkt 1

HCID 65577Trioctylphosphine oxide

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 962WaterLösungsmittelHCID 3283Diethyl EtherLösungsmittelHCID 7237O-XyleneLösungsmittel

Versuchsvorschrift

A solution of 44.5 g of octyl chloride in 300 cc of xylene was added dropwise to 12 g of degreased and dry magnesium immersed in a few cc of anhydrous diethyl ether, whilst heating until the reaction started. When the reaction had started, the octyl chloride was added in the cold. When all the octyl chloride solution had been added, stirring was continued for about 1 hour further. 13.8 g of phosphorus oxychloride were then added in the cold. The mixture was then heated to boiling under reflux for 2 hours 30 minutes. The solution was hydrolysed by the addition of 1 litre of water acidified with 100 cc of HCl. The organic phase was decanted, washed with distilled water and neutralised with sodium bicarbonate. After decanting, the organic phase was recovered and then steam-distilled or steam-stripped to remove the solvent without distilling the product. A white solid, trioctylphosphine oxide, was obtained.

Aufarbeitung

  1. temperaturewhilst heating until the reaction
  2. temperatureThe mixture was then heated
  3. temperatureunder reflux for 2 hours 30 minutes
  4. customThe organic phase was decanted
  5. washwashed with distilled water and neutralised with sodium bicarbonate
  6. customAfter decanting
  7. customthe organic phase was recovered
  8. distillationsteam-distilled
  9. customsteam-stripped to remove the solvent
  10. distillationwithout distilling the product

Quellen und Nachweise

ORD-Eintrag
ord-3741f59304ce4119a7336812e3a2b051
Quelldatensatz
uspto-grants-1976_01
Patentnummer
US03932524

Verknüpfte Notizen

Wird geladen…