Pyrazole → 1-Phenyl-2-(1H-pyrazol-1-yl)ethanone

HRID 133474

反応式

HRID 133474 の反応式
Cl[CH2:2][C:3]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)=[O:4].[NH:11]1[CH:15]=[CH:14][CH:13]=[N:12]1.C([O-])([O-])=O.[K+].[K+]>CC#N.CCOC(C)=O>[C:5]1([C:3](=[O:4])[CH2:2][N:11]2[CH:15]=[CH:14][CH:13]=[N:12]2)[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1

参加物

6

反応物 3

HCID 1048PyrazoleHCID 107572-ChloroacetophenoneHCID 11430Potassium Carbonate

生成物 1

HCID 27663751-Phenyl-2-(1H-pyrazol-1-yl)ethanone

試薬・触媒・溶媒 2

HCID 6342Acetonitrile溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 1.5 g (9.7 mmol) of 2-chloroacetophenone in 10 mL of MeCN, 0.7 g (10.3 mmol) of pyrazole was added. After all the solids dissolved, 1.4 g (10.1 mmol) of ground K2CO3 was added and the mixture was stirred for 5 h. The reaction was diluted with EtOAc, filtered, and the solid was washed with EtOAc. The filtrate was washed with water and brine, then was dried and concentrated. The residue was chromatographed on a flash column using a gradient of 10-50% EtOAc-hexane to isolate desired product.

後処理

  1. dissolutionAfter all the solids dissolved
  2. filtrationfiltered
  3. washthe solid was washed with EtOAc
  4. washThe filtrate was washed with water and brine
  5. customwas dried
  6. concentrationconcentrated
  7. customThe residue was chromatographed on a flash column

出典と根拠

ORDレコード
ord-1eabe1ca28e24df185018b6299bd77d2
出典データセット
uspto-grants-2008_06
特許番号
US07390835B2

関連ノート

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