HCID 20435938, Verbindung → HCID 20435958, Verbindung

HRID 1154038Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1154038
I[CH2:2][CH2:3][C:4]1([CH3:19])[C:16](=[O:17])[N:7]2[CH2:8][CH:9]=[CH:10][CH:11]([C:12]([O:14][CH3:15])=[O:13])[N:6]2[C:5]1=[O:18].[C:20]([O-:23])(=[S:22])[CH3:21].[K+]>CC(C)=O>[C:20]([S:22][CH2:2][CH2:3][C:4]1([CH3:19])[C:16](=[O:17])[N:7]2[CH2:8][CH:9]=[CH:10][CH:11]([C:12]([O:14][CH3:15])=[O:13])[N:6]2[C:5]1=[O:18])(=[O:23])[CH3:21]

Komponenten

4

Edukt 2

HCID 20435938HCID 20435938, VerbindungHCID 23670855Potassium ethanethioate

Produkt 1

HCID 20435958HCID 20435958, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Versuchsvorschrift

A mixture of 6.43 g (17 mmol) of methyl 2,3,5,8-tetrahydro-2-(2-iodoethyl)-2-methyl-1,3-dioxo-1H-pyrazolo-[1,2-a]pyridazine-5-carboxylate and 1.94 g (17 mmol) of potassium thioacetate in 150 ml of acetone was stirred at room temperature for 5 hours. The solvent was removed by evaporation and the residue was partitioned between dichloromethane and water. The organic phase was separated, dried over magnesium sulfate and evaporated to give methyl 2-(2-acetylthioethyl)-2,3,5,8-tetrahydro-2-methyl-1,3-dioxo-1H-pyrazolo[1,2-a]pyridazine-5-carboxylate as a mixture of diastereomers. Chromatography on silica gel using diethyl ether for the elution gave 3.81 g (69%) of diastereomer A in the form of a colorless oil and 1.26 g (23%) of diastereomer B in the form of a colorless oil.

Aufarbeitung

  1. customThe solvent was removed by evaporation
  2. customthe residue was partitioned between dichloromethane and water
  3. customThe organic phase was separated
  4. dry with materialdried over magnesium sulfate
  5. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-83365bed99c5426eb7831fa2567c86a2
Quelldatensatz
uspto-grants-1984_12
Patentnummer
US04487929

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