Ammonia → Phosphinic acid, (3-aminopropyl)(diethoxymethyl)-, ethyl ester

HRID 5164

Reaktionsgleichung

Reaktionsgleichung von HRID 5164
[C:1]([CH2:3][CH2:4][P:5]([CH:10]([O:14][CH2:15][CH3:16])[O:11][CH2:12][CH3:13])(=[O:9])[O:6][CH2:7][CH3:8])#[N:2].N.[H][H]>C(O)C.[Ni]>[NH2:2][CH2:1][CH2:3][CH2:4][P:5]([CH:10]([O:14][CH2:15][CH3:16])[O:11][CH2:12][CH3:13])(=[O:9])[O:6][CH2:7][CH3:8]

Komponenten

6

Edukt 3

HCID 222AmmoniaHCID 10037677Ethyl 2-cyanoethyl(diethoxymethyl)phosphinateHCID 178418361HCID 178418361, Verbindung

Produkt 1

HCID 10422382Phosphinic acid, (3-aminopropyl)(diethoxymethyl)-, ethyl ester

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 935NickelKatalysatorHCID 702EthanolLösungsmittel2×

Versuchsvorschrift

A solution of 9.6 g of ethyl 2-cyanoethyl(diethoxymethyl)phosphinate in 450 ml of ethanol is added to 82 g of an 8% solution of ammonia in ethanol. To this is added 5 ml of Raney Nickel and the resulting mixture is hydrogenated at 1 bar until the theoretical amount of hydrogen has been taken up. The mixture is then filtered, the filtrate is concentrated under reduced pressure and the crude product is distilled to give ethyl 3-aminopropyl(diethoxymethyl)phosphinate, b.p. 150° C./0.01 mbar, 31P=+46.4 ppm (CDCl3).

Aufarbeitung

  1. filtrationThe mixture is then filtered
  2. concentrationthe filtrate is concentrated under reduced pressure
  3. distillationthe crude product is distilled

Quellen und Nachweise

ORD-Eintrag
ord-ef2495e77e554402bda2035c66f5f24f
Quelldatensatz
uspto-grants-1993_09
Patentnummer
US05243062

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