Ibudilast → 2-Isopropylpyrazolo[1,5-a]pyridine

HRID 436802

反応式

HRID 436802 の反応式
[CH:1]([C:4]1[C:12](C(=O)C(C)C)=[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][N:6]2[N:5]=1)([CH3:3])[CH3:2].[OH-].[Na+]>S(=O)(=O)(O)O>[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]

参加物

4

反応物 2

HCID 3671IbudilastHCID 14798Sodium Hydroxide

生成物 1

HCID 113786582-Isopropylpyrazolo[1,5-a]pyridine

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

反応条件

温度
140 °C

実験手順

A mixture of 30g (0.13 mole) of 2-isopropyl-3-isobutyrylpyrazolo[1,5-a]pyridine and 200 ml of 50% sulfuric acid (v/v) solution was heated at 140° C for 10 hours. After cooling, the mixture was added to 400g of ice-water. The solution was neutralized with sodium hydroxide solution and extracted with chloroform. The chloroform solution was dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue was distilled to give 8.5g (5.3 × 10-2 mole) of colorless oily product, bp 127.5°-129.5° C (17 mmHg).

後処理

  1. temperatureAfter cooling
  2. extractionextracted with chloroform
  3. dry with materialThe chloroform solution was dried over anhydrous sodium sulfate
  4. concentrationconcentrated under reduced pressure
  5. distillationThe residue was distilled

出典と根拠

ORDレコード
ord-aff47afc56f346a5aa54cc804b107b9b
出典データセット
uspto-grants-1977_06
特許番号
US04028370

関連ノート

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