Hydrochloric Acid → Trioctylphosphine oxide

HRID 1580330

반응식

HRID 1580330 반응식
[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]

참가 물질

8

반응물 4

HCID 313Hydrochloric AcidHCID 81421-Chlorooctane3회HCID 24813Phosphorus oxychlorideHCID 5462224Magnesium

생성물 1

HCID 65577Trioctylphosphine oxide

시약·촉매·용매 3

HCID 962Water용매HCID 3283Diethyl Ether용매HCID 7237O-Xylene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3741f59304ce4119a7336812e3a2b051
출처 데이터셋
uspto-grants-1976_01
특허 번호
US03932524

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