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Ammonium Hydroxide → 2-(3-Mercapto-1-oxopropyl)-5-oxo-3-pyrazolidinecarboxylic acid

HRID 27261
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 27261
C([S:4][CH2:5][CH2:6][C:7]([N:9]1[CH:13]([C:14]([OH:16])=[O:15])[CH2:12][C:11](=[O:17])[NH:10]1)=[O:8])(=O)C.[OH-].[NH4+]>>[SH:4][CH2:5][CH2:6][C:7]([N:9]1[CH:13]([C:14]([OH:16])=[O:15])[CH2:12][C:11](=[O:17])[NH:10]1)=[O:8]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

3

Edukt 2

HCID 14923Ammonium HydroxideHCID 23344444HCID 23344444, Verbindung

Produkt 1

HCID 233444412-(3-Mercapto-1-oxopropyl)-5-oxo-3-pyrazolidinecarboxylic acidAusbeute 44,7 %

Versuchsvorschrift

DL-2-[3-(Acetylthio)-1-oxopropyl]-5-oxo-3-pyrazolidinecarboxylic acid (1.2 g) is treated in an argon atmosphere with 8 ml of a cold solution of 6.5 N ammonium hydroxide. After one hour at room temperature, the solution is extracted with ethyl acetate and treated with concentrated hydrochloric acid to pH 2. The water soluble product is extracted with five 20 ml portions of ethyl acetate. The combined extracts are dried over magnesium sulfate and evaporated to an oil which gradually solidifies. This material is dried in vacuo at 100° C. for 1 hour yielding 0.45 g of the title compound, melting point 140°-142° C.

Aufarbeitung

extraction
the solution is extracted with ethyl acetate
  • additiontreated with concentrated hydrochloric acid to pH 2
  • extractionThe water soluble product is extracted with five 20 ml portions of ethyl acetate
  • dry with materialThe combined extracts are dried over magnesium sulfate
  • customevaporated to an oil which
  • customThis material is dried in vacuo at 100° C. for 1 hour
  • Quellen und Nachweise

    ORD-Eintrag
    ord-39f6373776314ee2a372f4309ef8097e
    Quelldatensatz
    uspto-grants-1980_09
    DOI
    10.6084/m9.figshare.5104873.v1
    Patentnummer
    US04220791

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