Hydrazine hydrate (1:1) → 1-Methyl-2-oxo-1,2-dihydropyridine-4-carbohydrazide

HRID 500550Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 500550
C[O:2][C:3]([C:5]1[CH:10]=[CH:9][N:8]([CH3:11])[C:7](=[O:12])[CH:6]=1)=O.O.[NH2:14][NH2:15]>C(O)C.C(OCC)C>[CH3:11][N:8]1[CH:9]=[CH:10][C:5]([C:3]([NH:14][NH2:15])=[O:2])=[CH:6][C:7]1=[O:12]

Komponenten

5

Edukt 2

HCID 24654Hydrazine hydrate (1:1)HCID 819408Methyl 1-methyl-2-oxo-1,2-dihydropyridine-4-carboxylate

Produkt 1

HCID 431322131-Methyl-2-oxo-1,2-dihydropyridine-4-carbohydrazideAusbeute 78 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 3283Diethyl EtherLösungsmittel

Reaktionsbedingungen

Temperatur
78 °C

Versuchsvorschrift

The title compound from example 30.1 (4 g, 24 mmol) was dissolved in ethanol and stirred at 78° C. Hydrazine hydrate (5.8 mL, 120 mmol) was added via a syringe and the reaction was stirred for 3 h at 78° C., at which time the starting material was no longer visible by TLC. The reaction mixture (clear solution) was then cooled to room temperature, and diluted with diethyl ether to precipitate the product which was collected by vacuum filtration to yield the title compound as a pale yellow solid (3.13 g, 78%).

Aufarbeitung

  1. stirringthe reaction was stirred for 3 h at 78° C., at which time the starting material
  2. temperatureThe reaction mixture (clear solution) was then cooled to room temperature
  3. customto precipitate the product which
  4. filtrationwas collected by vacuum filtration

Quellen und Nachweise

ORD-Eintrag
ord-e1a49d0a4fd34ae4a7b28283f5fd8679
Quelldatensatz
uspto-grants-2010_08
Patentnummer
US07772235B2

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