Sodium Carbonate → Diisobutylphosphinic acid
Reaction equation
C([O-])([O-])=O.[Na+].[Na+].[CH2:7]([PH:11](=[O:13])[OH:12])[CH:8]([CH3:10])[CH3:9]>>[CH2:7]([P:11]([CH2:7][CH:8]([CH3:10])[CH3:9])(=[O:12])[OH:13])[CH:8]([CH3:10])[CH3:9]Participants
3
Procedure
The concentration of acid was determined by 31P NMR. 10% Na2CO3 solution was prepared in an amount sufficient to neutralize monoisobutylphosphinic acid. The oily fraction in the wash tank was washed with Na2CO3 solution in several portions each time separating the bottom aqueous layer from the wash tank. When removal of sodium monoisobutylphosphinate was completed, as monitored by 13P NMR, the additional water wash was performed on the remaining diisobutylphosphinic acid. The remaining water and toluene were removed under vacuum.
Workup
- customwas prepared in an amount sufficient
- washThe oily fraction in the wash tank was washed with Na2CO3 solution in several portions each time
- customseparating the bottom aqueous layer from the wash tank
- customWhen removal of sodium monoisobutylphosphinate
- washthe additional water wash
- customThe remaining water and toluene were removed under vacuum
Sources & evidence
- ORD record
- ord-d9ff383e7eb642159b65ef46d57240b4
- Source dataset
- uspto-grants-2011_08
- Patent number
- US08003722B2
Reaction notes
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