Lithium hydroxide, monohydrate → HCID 19430093, Verbindung

HRID 483990Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 483990
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

Komponenten

5

Edukt 2

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

Produkt 1

HCID 19430093HCID 19430093, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

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°.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-f5bbf235c3a34f72a8f55c98252e52b6
Quelldatensatz
uspto-grants-1993_07
Patentnummer
US05229379

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