Acetic Anhydride → Diethyl[3-(acetylamino)propyl]phosphonate

HRID 437048

Reaktionsgleichung

Reaktionsgleichung von HRID 437048
[CH2:1]([O:3][P:4]([CH2:9][CH2:10][CH2:11][NH2:12])(=[O:8])[O:5][CH2:6][CH3:7])[CH3:2].[C:13](OC(=O)C)(=[O:15])[CH3:14]>N1C=CC=CC=1>[CH2:6]([O:5][P:4]([CH2:9][CH2:10][CH2:11][NH:12][C:13](=[O:15])[CH3:14])(=[O:8])[O:3][CH2:1][CH3:2])[CH3:7]

Komponenten

4

Edukt 2

HCID 7918Acetic AnhydrideHCID 78113Diethyl (3-aminopropyl)phosphonate

Produkt 1

HCID 254237Diethyl[3-(acetylamino)propyl]phosphonateAusbeute 96 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

97 g. of 3-aminopropanephosphonic acid diethyl ester is dissolved in 400 ml. of dry pyridine and 55 g. of acetic anhydride is added with stirring. The mixture is then boiled for 4 hours with refluxing and freed of the low-boiling components by evaporation in a light vacuum. Gaschromatographically pure N-acetyl-3-aminopropanephosphonic acid diethyl ester is obtained in a 96% yield by shortcut distillation in vacuo. It is a pale yellow, highly viscous oil with a boiling point of 166° to 160° C. (0.4 Torr).

Aufarbeitung

  1. temperaturewith refluxing
  2. customfreed of the low-boiling components by evaporation in a light vacuum

Quellen und Nachweise

ORD-Eintrag
ord-9844bdada756410ba5bfbd9cd3a8f9a3
Quelldatensatz
uspto-grants-1977_06
Patentnummer
US04029679

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