2-Methylpyrazolo[1,5-a]pyridine-5-carboxylic acid → HCID 22388192、化合物

HRID 1699800ノート

反応式

HRID 1699800 の反応式
[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

参加物

3

反応物 2

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

生成物 1

HCID 22388192HCID 22388192、化合物

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-0eb74a558249448293b4f2fb16b77954
出典データセット
uspto-grants-2002_02
特許番号
US06348474B1

反応ノート

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