2-Oxo-2-(4-(trifluoromethyl)phenyl)acetaldehyde → 1-[4-hydroxy-1-methyl-5-(4-trifluoromethylphenyl)-1H-pyrazol-3-yl]ethanone

HRID 1881565ノート

反応式

HRID 1881565 の反応式
[CH3:1][NH:2][N:3]=[CH:4][C:5](=[O:7])[CH3:6].[F:8][C:9]([F:21])([F:20])[C:10]1[CH:15]=[CH:14][C:13]([C:16](=O)[CH:17]=[O:18])=[CH:12][CH:11]=1>C(O)(=O)C>[F:8][C:9]([F:21])([F:20])[C:10]1[CH:15]=[CH:14][C:13]([C:16]2[N:2]([CH3:1])[N:3]=[C:4]([C:5](=[O:7])[CH3:6])[C:17]=2[OH:18])=[CH:12][CH:11]=1

参加物

4

反応物 2

HCID 27832862-Oxo-2-(4-(trifluoromethyl)phenyl)acetaldehydeHCID 727702682-Oxopropanal methylhydrazone

生成物 1

HCID 602067901-[4-hydroxy-1-methyl-5-(4-trifluoromethylphenyl)-1H-pyrazol-3-yl]ethanone収率 8.6%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
100 °C

実験手順

2-Oxopropanal methylhydrazone (8.540 mmol, 855 mg) synthesized in Reference Synthetic Example 1 and (4-trifluoromethylphenyl)(oxo)acetaldehyde (6.432 mmol, 1.3 g) synthesized in Reference Synthetic Example 7 were dissolved in acetic acid (30 mL) and stirred at 100° C. for about 5 hours. Then, the solvent was evaporated, and the residue was dried by means of a vacuum pump and purified by silica gel column chromatography (n-hexane/AcOEt=2/1, and 4/1) to give the desired product as an orange solid (157.3 mg, yield 8.6%).

後処理

  1. customsynthesized in Reference Synthetic Example 7
  2. customThen, the solvent was evaporated
  3. customthe residue was dried by means of a vacuum pump
  4. custompurified by silica gel column chromatography (n-hexane/AcOEt=2/1, and 4/1)

出典と根拠

ORDレコード
ord-33aa5fad2bf44cfbb3d6323a59d61754
出典データセット
uspto-grants-2012_11
特許番号
US08318796B2

反応ノート

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