Ammonia → Ethyl 3-amino-1-methylpropyl(diethoxymethyl)phosphinate

HRID 2209925Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2209925
[CH3:1][CH:2]([P:6]([CH:11]([O:15][CH2:16][CH3:17])[O:12][CH2:13][CH3:14])(=[O:10])[O:7][CH2:8][CH3:9])[CH2:3][C:4]#[N:5].N.[H][H]>C(O)C.[Ni]>[NH2:5][CH2:4][CH2:3][CH:2]([P:6]([CH:11]([O:15][CH2:16][CH3:17])[O:12][CH2:13][CH3:14])(=[O:10])[O:7][CH2:8][CH3:9])[CH3:1]

Komponenten

6

Edukt 3

HCID 222AmmoniaHCID 14362805Ethyl 1-methyl-2-cyanoethyl(diethoxymethyl)phosphinateHCID 178418361HCID 178418361, Verbindung

Produkt 1

HCID 14362808Ethyl 3-amino-1-methylpropyl(diethoxymethyl)phosphinate

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 935NickelKatalysatorHCID 702EthanolLösungsmittel2×

Versuchsvorschrift

A solution of 17.0 g of ethyl 1-methyl-2-cyanoethyl(diethoxymethyl)phosphinate in 150 ml of ethanol is added to 155.0 g of an 8% solution of ammonia in ethanol. To this are added 10 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 and the filtrate is concentrated under reduced pressure and the crude product is distilled under reduced pressure to give ethyl 3-amino-1-methylpropyl(diethoxymethyl)phosphinate, b.p. 140° C./0.01 mbar, 31 p=+47.0 and +46.7 ppm (CDCl3).

Aufarbeitung

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

Quellen und Nachweise

ORD-Eintrag
ord-d55f7dfb69804d478d76593c98c4194f
Quelldatensatz
uspto-grants-1995_10
Patentnummer
US05457095

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