Lithium hydroxide, monohydrate → HCID 19430093, compound

HRID 1654459Notes

Reaction equation

HRID 1654459 reaction equation
O.[OH-].[Li+].C([O:6][P:7]([CH2:16][CH2:17][CH2:18][NH:19][CH2:20][C:21]1[CH:26]=[CH:25][C:24]([Cl:27])=[CH:23][CH:22]=1)([CH:9]([O:13][CH2:14][CH3:15])[O:10][CH2:11][CH3:12])=[O:8])C>O.C(O)C>[Cl:27][C:24]1[CH:23]=[CH:22][C:21]([CH2:20][NH: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])=[CH:26][CH:25]=1

Participants

5

Reactant 2

HCID 168937Lithium hydroxide, monohydrateHCID 544329463-(p-Chlorobenzylamino)propyl(diethoxymethyl)phosphinic acid ethyl ester

Product 1

HCID 19430093HCID 19430093, compound

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 962WaterSolvent

Procedure

A solution of 0.36 g of lithium hydroxide monohydrate in 7 ml of water is added to a solution of 1.61 g of 3-(p-chlorobenzylamino)propyl(diethoxymethyl)phosphinic acid ethyl ester in 3 ml of ethanol, and the mixture is heated at 60° for 24 hours. The mixture is then cooled to room temperature and the solvent is removed under reduced pressure. The evaporation residue is taken up in water and neutralised with phosphoric acid. A white precipitate forms and is filtered off, and the filtrate is concentrated to dryness by evaporation. The white residue is dried under reduced pressure and crystallised from toluene/diethyl ether. Filtration with suction and drying yield 3-(p-chlorobenzylamino)propyl(diethoxymethyl)phosphinic acid having a melting point of 177°-179°.

Workup

  1. temperaturethe mixture is heated at 60° for 24 hours
  2. customthe solvent is removed under reduced pressure
  3. filtrationA white precipitate forms and is filtered off
  4. concentrationthe filtrate is concentrated to dryness by evaporation
  5. customThe white residue is dried under reduced pressure
  6. customcrystallised from toluene/diethyl ether
  7. filtrationFiltration with suction
  8. customdrying

Sources & evidence

ORD record
ord-ed3d104700b44561916862a325d79df9
Source dataset
uspto-grants-1995_04
Patent number
US05407922

Reaction notes

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