Ammonia → HCID 18780195, compound

HRID 1421652Notes

Reaction equation

HRID 1421652 reaction equation
[CH2:1]([OH:3])[CH3:2].N.Cl[P:6]([CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1>>[CH2:13]([P:6]([C:7]1[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=1)[O:3][CH2:1][CH3:2])[CH2:14][CH2:15][CH2:16][CH2:17][CH3:18]

Participants

4

Reactant 3

HCID 222AmmoniaHCID 702EthanolHCID 18780192HCID 18780192, compound

Product 1

HCID 18780195HCID 18780195, compoundYield 79.2%

Procedure

135 g (2.94 mol) of absolute ethanol are cooled to -15° C. under a nitrogen atmosphere. 7.4 g (0.435 mol) of ammonia are then introduced at this temperature with constant stirring. 86 g (0.376 mol) of chloro-(n-hexyl)phenyl-phosphine are then added dropwise at this temperature in 40 minutes, then the mixture is allowed to come to room temperature with stirring, is filtered by suction and washed with ethanol. The filtrate is freed from ethanol and any ammonia present in vacuo. The remaining residue is distilled. 71 g of ethyl n-hexyl(phenyl)phosphinite are obtained at 1.1 mbar and an overhead temperature of 110° C. This corresponds to a yield of 79% of theory.

Workup

  1. customto come to room temperature
  2. filtrationis filtered by suction
  3. washwashed with ethanol
  4. distillationThe remaining residue is distilled

Sources & evidence

ORD record
ord-7d10dd34e579460d927abd989fba7ef4
Source dataset
uspto-grants-2000_06
Patent number
US06077968

Reaction notes

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