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Sodium Phosphate, Dibasic → HCID 20435948, Verbindung

HRID 1154054
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1154054
C([S:4][CH2:5][CH:6]1[CH2:17][N:9]2[CH2:10][CH2:11][CH2:12][CH:13]([C:14]([OH:16])=[O:15])[N:8]2[C:7]1=[O:18])(=O)C.P([O-])([O-])(O)=O.[Na+].[Na+]>Cl>[SH:4][CH2:5][CH:6]1[CH2:17][N:9]2[CH2:10][CH2:11][CH2:12][CH:13]([C:14]([OH:16])=[O:15])[N:8]2[C:7]1=[O:18]
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Komponenten

4

Edukt 2

HCID 24203Sodium Phosphate, DibasicHCID 204359472-acetylthiomethyl-hexahydro-3-oxo-1H-pyrazolo[1,2-a]pyridazine-5-carboxylic acid

Produkt 1

HCID 20435948HCID 20435948, VerbindungAusbeute 72,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 313Hydrochloric AcidLösungsmittel

Versuchsvorschrift

1.8 g of 2-acetylthiomethyl-hexahydro-3-oxo-1H-pyrazolo[1,2-a]pyridazine-5-carboxylic acid were heated at 95° C. for 1.5 hours in 2 M hydrochloric acid. The mixture was cooled, the pH was adjusted to 3 by the addition of disodium hydrogen orthophosphate and the aqueous solution was extracted repeatedly with ethyl acetate. The organic extracts were dried over magnesium sulfate and evaporated. After recrystallization of the residue from acetone, there were obtained 1.1 g of hexahydro-2-mercaptomethyl-3-oxo-1H- pyrazolo[1,2-a]pyridazine-5-carboxylic acid having a melting point of 145.5°-147° C.

Aufarbeitung

  1. temperatureThe mixture was cooled
  2. extractionthe aqueous solution was extracted repeatedly with ethyl acetate
  3. dry with materialThe organic extracts were dried over magnesium sulfate
  4. customevaporated
  5. customAfter recrystallization of the residue from acetone

Quellen und Nachweise

ORD-Eintrag
ord-83caaa74b49243c0bf428075d0915044
Quelldatensatz
uspto-grants-1984_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04487929

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