Hydrogen Peroxide → Sec.-butyl-di-n-octyl phosphine oxide

HRID 476778Notes

Reaction equation

HRID 476778 reaction equation
[OH:1]O.[CH:3]([P:7]([CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH3:23])[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH3:15])([CH2:5][CH3:6])[CH3:4]>O>[CH:3]([P:7](=[O:1])([CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH3:23])[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH3:15])([CH2:5][CH3:6])[CH3:4]

Participants

4

Reactant 2

HCID 784Hydrogen PeroxideHCID 14121815Sec.-butyl-di-n-octyl phosphine

Product 1

HCID 14094216Sec.-butyl-di-n-octyl phosphine oxide

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
70 °C

Procedure

40 g H2O2 (0.35 mol, 30% solution) was added dropwise while cooling with water and with intense agitation to 80 g (0.25 mol) sec.-butyl-di-n-octyl phosphine in a 500 ml-double-walled vessel. After all had been added, the reaction solution was heated to 70° C. over a period of 30 minutes, while stirring was interrupted. An aqueous phase which deposited on the bottom of the vessel was separated. It was admixed with 4.5 ml sodium carbonate solution (30 g/l) and the pH increased from 5.6 to 9.2. The whole was stirred over a period of 1 hour at 80° C. and allowed to deposit. The aqueous phase was separated and the crude product was distilled in vacuum.

Workup

  1. additionAfter all had been added
  2. customwas separated
  3. temperaturethe pH increased from 5.6 to 9.2
  4. stirringThe whole was stirred over a period of 1 hour at 80° C.
  5. customThe aqueous phase was separated
  6. distillationthe crude product was distilled in vacuum

Sources & evidence

ORD record
ord-bf0cb5c36d3f4a46865e800160090ebd
Source dataset
uspto-grants-1989_12
Patent number
US04885393

Reaction notes

Loading…