HCID 67828048, compound → 3-Aminopropyl-cyclohexylmethylphosphinic acid

HRID 1612699Notes

Reaction equation

HRID 1612699 reaction equation
Cl.[NH2:2][CH2:3][CH2:4][CH2:5][P:6]([CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)(=[O:8])[OH:7]>CO>[NH2:2][CH2:3][CH2:4][CH2:5][P:6]([CH2:9][CH:10]1[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]1)(=[O:7])[OH:8]

Participants

3

Reactant 1

HCID 67828048HCID 67828048, compound

Product 1

HCID 1300223-Aminopropyl-cyclohexylmethylphosphinic acid

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

A mixture of 3.0 g of 3-aminopropyl(benzyl)phosphinic acid hydrochloride and 0.6 g of Nishimura catalyst in 30 ml of methanol is hydrogenated during 4 hours. The catalyst is filtered off and the solvent removed by evaporation. The residue is dissolved in 20 ml of methanol and 10 ml of propyleneoxide are added to the solution. Stirring for 3 hours affords a white solid which is filtered off and dried over phosphorous pentoxide to yield 3-aminopropyl(cyclohexylmethyl)phosphinic acid, m.p. 230° (dec.).

Workup

  1. filtrationThe catalyst is filtered off
  2. customthe solvent removed by evaporation
  3. dissolutionThe residue is dissolved in 20 ml of methanol
  4. addition10 ml of propyleneoxide are added to the solution
  5. customaffords a white solid which
  6. filtrationis filtered off
  7. dry with materialdried over phosphorous pentoxide

Sources & evidence

ORD record
ord-a7752df201f34bcb8b9841524ba6c513
Source dataset
uspto-grants-1993_03
Patent number
US05190933

Reaction notes

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