Acetic Anhydride → 1-(2-Phenylpyrazolo[1,5-a]pyridin-3-yl)-1-ethanone

HRID 487618

反応式

HRID 487618 の反応式
[C:1]1([C:7]2[CH:15]=[C:10]3[CH:11]=[CH:12][CH:13]=[CH:14][N:9]3[N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:16](OC(=O)C)(=[O:18])[CH3:17]>S(=O)(=O)(O)O.[OH-].[Na+]>[C:1]1([C:7]2[C:15]([C:16](=[O:18])[CH3:17])=[C:10]3[CH:11]=[CH:12][CH:13]=[CH:14][N:9]3[N:8]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

5

反応物 2

HCID 7918Acetic AnhydrideHCID 156203422-Phenylpyrazolo[1,5-a]pyridine

生成物 1

HCID 107049561-(2-Phenylpyrazolo[1,5-a]pyridin-3-yl)-1-ethanone収率 47.7%

試薬・触媒・溶媒 2

HCID 1118Sulfuric Acid触媒HCID 14798Sodium Hydroxide溶媒

実験手順

2-Phenylpyrazolo[1,5-a]pyridine (2.00 g) was added to a stirred solution of acetic anhydride (4.20 g) and two drops of sulfuric acid at room temperature. After being stirred under reflux for 14 hours, the reaction mixture was poured onto 80 ml of 4N NaOH aqueous solution and extracted with chloroform (30 ml×2). The extracts were combined and washed with water (30 ml), saturated sodium chloride aqueous solution (30 ml), then dried over magnesium sulfate and evaporated in vacuo. The residual crystals were recrystallized from diisopropyl ether to give 2-phenyl-3-acetylpyrazolo-[1,5-a]pyridine (1.16 g).

後処理

  1. temperatureunder reflux for 14 hours
  2. extractionextracted with chloroform (30 ml×2)
  3. washwashed with water (30 ml), saturated sodium chloride aqueous solution (30 ml)
  4. dry with materialdried over magnesium sulfate
  5. customevaporated in vacuo
  6. customThe residual crystals were recrystallized from diisopropyl ether

出典と根拠

ORDレコード
ord-fd79c29a8ebc45e38ef16f04653cef91
出典データセット
uspto-grants-1994_03
特許番号
US05296490

関連ノート

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