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

HRID 436802

반응식

HRID 436802 반응식
[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]

참가 물질

4

반응물 2

HCID 3671IbudilastHCID 14798Sodium Hydroxide

생성물 1

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

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

반응 조건

온도
140 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-aff47afc56f346a5aa54cc804b107b9b
출처 데이터셋
uspto-grants-1977_06
특허 번호
US04028370

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