Lithium Hydroxide → 6-(Difluoromethyl)-2-oxo-1,2-dihydropyridine-3-carboxylic acid

HRID 512463Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 512463
[F:1][CH:2]([F:14])[C:3]1[NH:8][C:7](=[O:9])[C:6]([C:10]([O:12]C)=[O:11])=[CH:5][CH:4]=1.[OH-].[Li+]>CO.O>[F:14][CH:2]([F:1])[C:3]1[NH:8][C:7](=[O:9])[C:6]([C:10]([OH:12])=[O:11])=[CH:5][CH:4]=1

Komponenten

5

Edukt 2

HCID 3939Lithium HydroxideHCID 69233637HCID 69233637, Verbindung

Produkt 1

HCID 685011126-(Difluoromethyl)-2-oxo-1,2-dihydropyridine-3-carboxylic acid

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

7.4 g (36.4 mmol) of methyl 6-(difluoromethyl)-2-oxo-1,2-dihydropyridine-3-carboxylate were dissolved in 100 ml of methanol, and a solution of 1.3 g (54.6 mmol) of lithium hydroxide in 50 ml of water was added. After two hours of heating under reflux, the mixture was concentrated to a volume of about 50 ml and the solution was washed with dichloromethane. The aqueous phase was then acidified with 2N hydrochloric acid and extracted with ethyl acetate. Drying and concentration of the extract gave 5.6 g (82% of theory) of a brownish powder.

Aufarbeitung

  1. temperatureAfter two hours of heating
  2. temperatureunder reflux
  3. concentrationthe mixture was concentrated to a volume of about 50 ml
  4. washthe solution was washed with dichloromethane
  5. extractionextracted with ethyl acetate
  6. customDrying
  7. customconcentration of the extract gave 5.6 g (82% of theory) of a brownish powder

Quellen und Nachweise

ORD-Eintrag
ord-4f076c617179471f92cab9f88e7137f8
Quelldatensatz
uspto-grants-2015_08
Patentnummer
US09102623B2

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