反应详情

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.

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