Lithium Hydroxide → HCID 67326429, Verbindung

HRID 82477

Reaktionsgleichung

Reaktionsgleichung von HRID 82477
C[O:2][C:3](=[O:17])[C:4]([NH2:16])([C:8]([C:10]1[CH:11]=[N:12][CH:13]=[CH:14][CH:15]=1)=[O:9])[CH:5]([CH3:7])[CH3:6].C1COCC1.[Li+].[OH-]>CO.O>[CH3:6][CH:5]([CH3:7])[C:4]([NH2:16])([C:8]([C:10]1[CH:11]=[N:12][CH:13]=[CH:14][CH:15]=1)=[O:9])[C:3]([OH:17])=[O:2]

Komponenten

6

Edukt 3

HCID 3939Lithium HydroxideHCID 8028TetrahydrofuranHCID 673255273-Methyl-2-[pyridine-3-carbonyl]-amino-butyric acid methyl ester

Produkt 1

HCID 67326429HCID 67326429, VerbindungAusbeute 99 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
25 °C

Versuchsvorschrift

To a solution of 3-methyl-2-[pyridine-3-carbonyl]-amino-butyric acid methyl ester (1.5 g, 6.3 mmol), in methanol (15 mL), THF (9 mL) was added LiOH (1.3 g, 31.7 mmol) dissolved in water (3 mL). The mixture was allowed to stir at room temperature (25° C.) over 2 h. Solvent was evaporated from reaction mixture, dissolved in water (15 mL), acidified with 1.5N HCl extracted with ethyl acetate (150 mL), dried over sodium sulphate and concentrated to obtain product as yellow colour solid (1.38 g, 99%).

Aufarbeitung

  1. customSolvent was evaporated from reaction mixture
  2. dissolutiondissolved in water (15 mL)
  3. extractionextracted with ethyl acetate (150 mL)
  4. dry with materialdried over sodium sulphate
  5. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-15fe4b8c7f4a47eca4088ce693a8f5da
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08846721B2

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