Hydrazine hydrate (1:1) → (S)-3-[[(6-aminohexyl)ethoxyphosphinyl]amino]-2-oxo-1-piperidineacetic acid, ethyl ester

HRID 1285473Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1285473
[CH2:1]([O:3][P:4]([NH:23][C@H:24]1[CH2:29][CH2:28][CH2:27][N:26]([CH2:30][C:31]([O:33][CH2:34][CH3:35])=[O:32])[C:25]1=[O:36])([CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][N:12]1C(=O)C2=CC=CC=C2C1=O)=[O:5])[CH3:2].O.NN>O1CCOCC1.C1(C)C=CC=CC=1>[NH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][P:4]([NH:23][C@H:24]1[CH2:29][CH2:28][CH2:27][N:26]([CH2:30][C:31]([O:33][CH2:34][CH3:35])=[O:32])[C:25]1=[O:36])([O:3][CH2:1][CH3:2])=[O:5]

Komponenten

5

Edukt 2

HCID 24654Hydrazine hydrate (1:1)HCID 86740217(S)-3-[[ethoxy(6-phthalimidohexyl)phosphinyl]amino]-2-oxo-1-piperidineacetic acid, ethyl ester

Produkt 1

HCID 86740218(S)-3-[[(6-aminohexyl)ethoxyphosphinyl]amino]-2-oxo-1-piperidineacetic acid, ethyl ester

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 1140TolueneLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

A solution of (S)-3-[[ethoxy(6-phthalimidohexyl)phosphinyl]amino]-2-oxo-1-piperidineacetic acid, ethyl ester in dioxane is treated with hydrazine hydrate and stirred at room temperature under argon. After the reaction is completed, the mixture is diluted with toluene and the solvents decanted. The residue is triturated with methylene chloride and filtered. The combined filtrate is evaporated to dryness to give (S)-3-[[(6-aminohexyl)ethoxyphosphinyl]amino]-2-oxo-1-piperidineacetic acid, ethyl ester.

Aufarbeitung

  1. customthe solvents decanted
  2. customThe residue is triturated with methylene chloride
  3. filtrationfiltered
  4. customThe combined filtrate is evaporated to dryness

Quellen und Nachweise

ORD-Eintrag
ord-6e11aecd3f0a490cb7bc9efb294199dd
Quelldatensatz
uspto-grants-1986_01
Patentnummer
US04567167

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