Ammonia → HCID 18780198, compound

HRID 1421653Notes

Reaction equation

HRID 1421653 reaction equation
[CH2:1]([OH:3])[CH3:2].N.[C:5]1([P:11]([CH:13]([CH3:15])[CH3:14])Cl)[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1>>[CH:13]([P:11]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)[O:3][CH2:1][CH3:2])([CH3:15])[CH3:14]

Participants

4

Reactant 3

HCID 222AmmoniaHCID 702EthanolHCID 10867074HCID 10867074, compound

Product 1

HCID 18780198HCID 18780198, compoundYield 85%

Procedure

50 g (1.09 mol) of absolute ethanol are cooled to -15° C. under a nitrogen atmosphere. 3 g (1.76 mol) of ammonia gas are then introduced at this temperature with constant stirring. 26 g (1.39 mol) of phenyl(isopropyl)chloro-phosphine are then added dropwise at this temperature in 30 minutes. The mixture is then stirred for a further 30 minutes at this temperature and then refluxed for a further 12 hours. The mixture is then cooled, filtered by suction and rinsed out with ethanol. The filtrate is freed from ethanol in vacuo and the remaining residue is distilled. 23 g of ethyl isopropyl(phenyl)phosphinite are obtained at 0.07 mbar and an overhead temperature of 50° C. This corresponds to a yield of 85% of theory.

Workup

  1. temperaturerefluxed for a further 12 hours
  2. temperatureThe mixture is then cooled
  3. filtrationfiltered by suction
  4. washrinsed out with ethanol
  5. distillationthe remaining residue is distilled

Sources & evidence

ORD record
ord-67b97ded82694632ae2e649edd3a5665
Source dataset
uspto-grants-2000_06
Patent number
US06077968

Reaction notes

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