HCID 67828048, compound → 3-Aminopropyl-cyclohexylmethylphosphinic acid

HRID 1463618Notes

Reaction equation

HRID 1463618 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-590f3e50d34c4f2fa959c05df511e2be
Source dataset
uspto-grants-1994_04
Patent number
US05300679

Reaction notes

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