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

HRID 1699800Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1699800
[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

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-0eb74a558249448293b4f2fb16b77954
Quelldatensatz
uspto-grants-2002_02
Patentnummer
US06348474B1

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