Lithium hydroxide, monohydrate → HCID 19748746, compound

HRID 484002Notes

Reaction equation

HRID 484002 reaction equation
O.[OH-].[Li+].C([O:6][P:7]([CH2:16][CH2:17][CH2:18][N:19]([CH2:21][C:22]1[CH:27]=[CH:26][C:25]([Cl:28])=[CH:24][CH:23]=1)[CH3:20])([CH:9]([O:13][CH2:14][CH3:15])[O:10][CH2:11][CH3:12])=[O:8])C>O.C(O)C>[Cl:28][C:25]1[CH:24]=[CH:23][C:22]([CH2:21][N:19]([CH2:18][CH2:17][CH2:16][P:7]([CH:9]([O:13][CH2:14][CH3:15])[O:10][CH2:11][CH3:12])(=[O:6])[OH:8])[CH3:20])=[CH:27][CH:26]=1

Participants

5

Reactant 2

HCID 168937Lithium hydroxide, monohydrateHCID 53959695HCID 53959695, compound

Product 1

HCID 19748746HCID 19748746, compound

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 962WaterSolvent

Procedure

0.43 g of lithium hydroxide monohydrate in 6 ml of water is added to a solution of 2.0 g of 3-[N-(p-chlorobenzyl)-N-methylamino]propyl(diethoxymethyl)phosphinic acid ethyl ester in 5.5 ml of ethanol, and the mixture is heated at 60° for 25 hours. The reaction mixture is cooled to room temperature, the solvent is removed under reduced pressure, and the evaporation residue is taken up in water and neutralised with phosphoric acid. The suspension formed is concentrated to dryness by evaporation, and the residue is taken up in hot methanol, filtered and concentrated by evaporation again. Crystallisation of the residue from propanol yields 3-[N-(p-chlorobenzyl)-N-methylamino]propyl(diethoxymethyl)phosphinic acid having a melting point of 170°-171.5°.

Workup

  1. temperaturethe mixture is heated at 60° for 25 hours
  2. customthe solvent is removed under reduced pressure
  3. customThe suspension formed
  4. concentrationis concentrated to dryness by evaporation
  5. filtrationfiltered
  6. concentrationconcentrated by evaporation again
  7. customCrystallisation of the residue from propanol

Sources & evidence

ORD record
ord-c4b9601625e44ec8946e9d688f26fca9
Source dataset
uspto-grants-1993_07
Patent number
US05229379

Reaction notes

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