2-Methylpyrazolo[1,5-a]pyridine-5-carboxylic acid → HCID 22388192, Verbindung

HRID 1072782Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1072782
[CH3:1][C:2]1[CH:13]=[C:5]2[CH:6]=[C:7]([C:10]([OH:12])=[O:11])[CH:8]=[CH:9][N:4]2[N:3]=1.S(=O)(=O)(O)O.[CH2:19](O)[CH3:20]>>[CH3:1][C:2]1[CH:13]=[C:5]2[CH:6]=[C:7]([C:10]([O:12][CH2:19][CH3:20])=[O:11])[CH:8]=[CH:9][N:4]2[N:3]=1

Komponenten

3

Edukt 2

HCID 223884352-Methylpyrazolo[1,5-a]pyridine-5-carboxylic acidHCID 73950302Sulphuric acid ethanol

Produkt 1

HCID 22388192HCID 22388192, Verbindung

Versuchsvorschrift

2-Methylpyrazolo[1,5-a]pyridine-5-carboxylic acid (723 mg) was dissolved in 10% sulfuric acid/ethanol (20 ml) and the mixture was refluxed under heating for 2.5 hr. The reaction mixture was neutralized under ice-cooling, extracted with ethyl acetate and dried over magnesium sulfate. The residue was concentrated to dryness under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=4:1) to give the objective compound (707 mg) as a pale-brown powder.

Aufarbeitung

  1. temperaturethe mixture was refluxed
  2. temperatureunder heating for 2.5 hr
  3. temperaturecooling
  4. extractionextracted with ethyl acetate
  5. dry with materialdried over magnesium sulfate
  6. concentrationThe residue was concentrated to dryness under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate=4:1)

Quellen und Nachweise

ORD-Eintrag
ord-b5955b54c40544ae8431a35eb0b9074c
Quelldatensatz
uspto-grants-2005_06
Patentnummer
US06911469B2

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