反応式
[NH:1]1[CH:5]=[CH:4][C:3]([CH:6]=[O:7])=[N:2]1.C(=O)([O-])[O-].[K+].[K+].[CH2:14](Br)[CH:15]=[CH2:16].O>CN(C=O)C>[CH2:16]([N:2]1[C:3]([CH:6]=[O:7])=[CH:4][CH:5]=[N:1]1)[CH:15]=[CH2:14]参加物
6
実験手順
Pyrazole-3-carbaldehyde (3.00 g, 31.2 mmol) was dissolved in DMF (20 ml), and thereto were added potassium carbonate (6.47 g, 46.8 mmol) and allyl bromide (3.50 g, 32.8 mmol) with stirring. The mixture was stirred at room temperature for 6 hours, and thereto was added water, and the mixture was extracted with ethyl acetate. The organic layer was washed with water and saturated saline, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the resulting residue was purified by silica gel column chromatography to give the title compound (429 mg, 10%).
後処理
- stirringThe mixture was stirred at room temperature for 6 hours
- extractionthe mixture was extracted with ethyl acetate
- washThe organic layer was washed with water and saturated saline
- dry with materialdried over anhydrous magnesium sulfate
- customThe solvent was evaporated under reduced pressure
- customthe resulting residue was purified by silica gel column chromatography
出典と根拠
- ORDレコード
- ord-fbfff4f61fb142d68d6b767e74c32fa3
- 出典データセット
- uspto-grants-2008_09
- 特許番号
- US07425642B2
関連ノート
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