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2-(4-(tert-Butyl)phenyl)-2-oxoacetaldehyde → 1-[5-(4-tert-butylphenyl)-1-ethyl-4-hydroxy-1H-pyrazol-3-yl]ethanone

HRID 2103824
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HRID 2103824 반응식
[CH2:1]([NH:3][N:4]=[CH:5][C:6](=[O:8])[CH3:7])[CH3:2].[C:9]([C:13]1[CH:18]=[CH:17][C:16]([C:19](=O)[CH:20]=[O:21])=[CH:15][CH:14]=1)([CH3:12])([CH3:11])[CH3:10]>C(O)(=O)C>[C:9]([C:13]1[CH:18]=[CH:17][C:16]([C:19]2[N:3]([CH2:1][CH3:2])[N:4]=[C:5]([C:6](=[O:8])[CH3:7])[C:20]=2[OH:21])=[CH:15][CH:14]=1)([CH3:12])([CH3:11])[CH3:10]
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참가 물질

4

반응물 2

HCID 135124882-(4-(tert-Butyl)phenyl)-2-oxoacetaldehydeHCID 860145522-Oxopropanal ethylhydrazone

생성물 1

HCID 670501791-[5-(4-tert-butylphenyl)-1-ethyl-4-hydroxy-1H-pyrazol-3-yl]ethanone수율 16%

시약·촉매·용매 1

HCID 176Acetic Acid용매

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온도
100 °C

실험 절차

2-Oxopropanal ethylhydrazone (4.736 mmol, 540.6 mg) synthesized in Reference Synthetic Example 2 and (4-tert-butylphenyl)(oxo)acetaldehyde (4.736 mmol, 901.0 mg) synthesized in Reference Synthetic Example 4 were dissolved in acetic acid (20 mL) and stirred at 100° C. for about 3.5 hours. Then, the solvent was evaporated, and the residue was dried by means of a vacuum pump and purified by silica gel thin layer chromatography (n-hexane/AcOEt=1/2, 3/1 and 4/1) to give the desired product as an orange liquid (212 mg, yield 16%).

후처리

  1. customsynthesized in Reference Synthetic Example 4
  2. customThen, the solvent was evaporated
  3. customthe residue was dried by means of a vacuum pump
  4. custompurified by silica gel thin layer chromatography (n-hexane/AcOEt=1/2, 3/1 and 4/1)

출처 및 근거

ORD 기록
ord-f57d1f63683b42ec805f85994fe22784
출처 데이터셋
uspto-grants-2009_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07576115B2

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