Acetic Anhydride → 1-[2-(Propan-2-yl)pyrazolo[1,5-a]pyridin-3-yl]ethan-1-one

HRID 839792ノート

反応式

HRID 839792 の反応式
[CH:1]([C:4]1[CH:12]=[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][N:6]2[N:5]=1)([CH3:3])[CH3:2].[C:13](OC(=O)C)(=[O:15])[CH3:14]>S(=O)(=O)(O)O.[OH-].[K+]>[C:13]([C:12]1[C:4]([CH:1]([CH3:3])[CH3:2])=[N:5][N:6]2[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=12)(=[O:15])[CH3:14]

参加物

5

反応物 2

HCID 7918Acetic AnhydrideHCID 113786582-Isopropylpyrazolo[1,5-a]pyridine

生成物 1

HCID 159338551-[2-(Propan-2-yl)pyrazolo[1,5-a]pyridin-3-yl]ethan-1-one収率 81.1%

試薬・触媒・溶媒 2

HCID 1118Sulfuric Acid触媒HCID 14797Potassium Hydroxide溶媒

実験手順

A mixture of 4.2g of 2-isopropylpyrazolo[1,5-a]-pyridine, 10.2g of acetic anhydride and 2-3 drops of concentrated sulfuric acid was refluxed for 7 hr. After cooling, the mixture was added to 200 ml of 4M potassium hydroxide solution and stirred for 1 hr. The solution was extracted with chloroform and the chloroform solution was dried over sodium sulfate. The dried chloroform solution was concentrated and the residue was columnchromatographed over alumina to isolate objective product. Recrystallization from n-hexane gave 4.3g of colorless needles, mp 74° C. Yield 67%.

後処理

  1. temperaturewas refluxed for 7 hr
  2. temperatureAfter cooling
  3. extractionThe solution was extracted with chloroform
  4. dry with materialthe chloroform solution was dried over sodium sulfate
  5. concentrationThe dried chloroform solution was concentrated
  6. customto isolate objective product
  7. customRecrystallization from n-hexane

出典と根拠

ORDレコード
ord-7501d1dc34534a46a42280ac97b4d82c
出典データセット
uspto-grants-1978_06
特許番号
US04097483

反応ノート

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