Sodium Phosphate, Dibasic → 1-Methyl-5-(methylthio)-1H-pyrazol-3-amine

Reaktionsgleichung

[NH2:1][C:2]1[C:6](C#N)=[C:5]([S:9][CH3:10])[N:4]([CH3:11])[N:3]=1.P([O-])([O-])(O)=O.[Na+].[Na+]>[OH-].[Na+]>[NH2:1][C:2]1[CH:6]=[C:5]([S:9][CH3:10])[N:4]([CH3:11])[N:3]=1

Komponenten

Reaktionsbedingungen

Temperatur: 50 °C

Versuchsvorschrift

5.55 g (33.0 mmol) 3-amino-4-cyano-1-methyl-5-methylmercaptopyrazole heated with 50 ml 32% caustic soda at boiling for 24 hours. The reaction mixture was cooled, made slightly acidic with aqueous sodium hydrogen phosphate, heated for 8 hours at 50° C. and extracted with ethyl acetate. The organic phase was dried over sodium sulfate, concentrated and the residue purified by silica gel chromatography (hexane/ethyl acetate 1:1).

Aufarbeitung

temperatureThe reaction mixture was cooled
extractionextracted with ethyl acetate
dry with materialThe organic phase was dried over sodium sulfate
concentrationconcentrated
customthe residue purified by silica gel chromatography (hexane/ethyl acetate 1:1)

Quellen und Nachweise

ORD-Eintrag: ord-c1a7f84277e14cdcbba2764d7cd70a90
Quelldatensatz: uspto-grants-1999_02
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US05869686

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Komponenten

Edukt 2

HCID 24203Sodium Phosphate, Dibasic

HCID 28195393-Amino-1-methyl-5-methylsulfanyl-1H-pyrazole-4-carbonitrile

Produkt 1

HCID 542284381-Methyl-5-(methylthio)-1H-pyrazol-3-amine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 14798Sodium HydroxideLösungsmittel