Sulfuric Acid → HCID 178454904, compound

HRID 1834545Notes

Reaction equation

HRID 1834545 reaction equation
[CH:1]([PH:5][O:6]CC)([CH2:3][CH3:4])[CH3:2].[CH2:9]([Mg]Br)[CH:10]([CH3:12])[CH3:11].OS(O)(=O)=O>O1CCCC1>[CH2:9]([PH:5](=[O:6])[CH:1]([CH2:3][CH3:4])[CH3:2])[CH:10]([CH3:12])[CH3:11]

Participants

5

Reactant 3

HCID 1118Sulfuric AcidHCID 20373792HCID 20373792, compoundHCID 178418816HCID 178418816, compound

Product 1

HCID 178454904HCID 178454904, compound

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent2×

Procedure

A solution of ethyl sec-butylphosphinite (25g., 0.17 mole) in tetrahydrofuran (50 ml.) was added dropwise to a cooled solution of iso-butyl magnesium bromide (0.4 mole) in tetrahydrofuran (150 ml.). The mixture was then heated under reflux for 18 hours. The mixture was then cooled, hydrolysed with 2N H2SO4, and extracted with methylene dichloride. The combined extracts were washed with NaHCO3 solution and then dried (MgSO4). The solvent was removed by distillation and the residue was distilled under reduced pressure to give isobutyl sec-butyl-phosphine oxide bp. 81°-3°/0.03 0.03 mm as a colourless liquid (yield 20g., 72%).

Workup

  1. temperatureThe mixture was then heated
  2. temperatureunder reflux for 18 hours
  3. extractionextracted with methylene dichloride
  4. washThe combined extracts were washed with NaHCO3 solution
  5. dry with materialdried (MgSO4)
  6. customThe solvent was removed by distillation
  7. distillationthe residue was distilled under reduced pressure

Sources & evidence

ORD record
ord-0ed4072233574041b345b6aadf6702d3
Source dataset
uspto-grants-1978_01
Patent number
US04070496

Reaction notes

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