HCID 13144528, Verbindung → HCID 13144530, Verbindung

HRID 1154039Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1154039
C([S:4][CH2:5][C:6]1([CH3:24])[C:21](=[O:22])[N:9]2[CH2:10][CH2:11][CH2:12][CH:13]([C:14]([O:16]C(C)(C)C)=[O:15])[N:8]2[C:7]1=[O:23])(=O)C>FC(F)(F)C(O)=O>[SH:4][CH2:5][C:6]1([CH3:24])[C:21](=[O:22])[N:9]2[CH2:10][CH2:11][CH2:12][CH:13]([C:14]([OH:16])=[O:15])[N:8]2[C:7]1=[O:23]

Komponenten

3

Edukt 1

HCID 13144528HCID 13144528, Verbindung

Produkt 1

HCID 13144530HCID 13144530, VerbindungAusbeute 43 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6422Trifluoroacetic acidLösungsmittel

Versuchsvorschrift

A solution of 0.71 g of tert.butyl 2-acetylthiomethyl-hexahydro-2-methyl1,3-dioxo-1H-pyrazolo[1,2-a]pyridazine-5-carboxylate (diastereomer A) in 10 ml of trifluoroacetic acid was left to stand at room temperature for 1 hour. The mixture was evaporated to dryness and the residue was stirred under nitrogen with 50 ml of 50:50 mixture of water and concentrated aqueous ammonia for 2 hours. The mixture was acified to pH 1 with hydrochloric acid, saturated with sodium chloride and extracted with chloroform. The chloroform extracts were dried over sodium sulfate and evaporated. The residue was recrystallized from ethyl acetate/hexane to give 0.22 g (43%) of hexahydro-2-mercaptomethyl-2-methyl-1,3-dioxo-1H-pyrazolo[1,2-a]pyridazine-5-carboxylic acid (diastereomer A) in the form of white crystals having a melting point of 209°-211° C.

Aufarbeitung

  1. customThe mixture was evaporated to dryness
  2. extractionextracted with chloroform
  3. dry with materialThe chloroform extracts were dried over sodium sulfate
  4. customevaporated
  5. customThe residue was recrystallized from ethyl acetate/hexane

Quellen und Nachweise

ORD-Eintrag
ord-f0a5c346f7084b82b686ea2488ff5470
Quelldatensatz
uspto-grants-1984_12
Patentnummer
US04487929

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