Methylhydrazine → Ethyl 2-(methylhydrazono)propanoate

HRID 422805

Reaktionsgleichung

Reaktionsgleichung von HRID 422805
[C:1]([O:6][CH2:7][CH3:8])(=[O:5])[C:2]([CH3:4])=O.[O-]S([O-])(=O)=O.[Mg+2].[CH3:15][NH:16][NH2:17]>C(Cl)(Cl)Cl>[CH3:15][NH:16][N:17]=[C:2]([CH3:4])[C:1]([O:6][CH2:7][CH3:8])=[O:5]

Komponenten

5

Edukt 3

HCID 6061MethylhydrazineHCID 12041Ethyl pyruvateHCID 24083Sulfuric acid magnesium salt (1:1)

Produkt 1

HCID 73828661Ethyl 2-(methylhydrazono)propanoateAusbeute 94 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel2×

Versuchsvorschrift

To a suspension of ethyl pyruvate (37.8 mL, 338 mmol) and MgSO4 (40.8 g, 339 mmol) in CHCl3 (500 mL) was added a solution of methylhydrazine (18.0 mL, 332 mmol) in CHCl3 (100 mL) at 0° C. The reaction mixture was warmed to room temperature. After stirring for 24 hours at room temperature, the reaction mixture was filtered. The filtrate was concentrated under reduced pressure to give 44 g (94%) of the desired product that was used directly without further purification.

Aufarbeitung

  1. filtrationthe reaction mixture was filtered
  2. concentrationThe filtrate was concentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-be115ec79c7245dd8fa5ab2a76317f7f
Quelldatensatz
uspto-grants-2012_01
Patentnummer
US08101639B2

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