反応式
[CH3:1][CH2:2][O:3][N:4]=[C:5]([C:8]1[C:13]([Cl:14])=[CH:12][C:11]([Cl:15])=[CH:10][N:9]=1)[CH2:6][NH2:7].C(N(CC)CC)C.[F:23][C:24]([F:35])([F:34])[C:25]1[CH:33]=[CH:32][CH:31]=[CH:30][C:26]=1[C:27](Cl)=[O:28].O>ClCCl>[Cl:14][C:13]1[C:8]([C:5](=[N:4][O:3][CH2:2][CH3:1])[CH2:6][NH:7][C:27](=[O:28])[C:26]2[CH:30]=[CH:31][CH:32]=[CH:33][C:25]=2[C:24]([F:23])([F:34])[F:35])=[N:9][CH:10]=[C:11]([Cl:15])[CH:12]=1参加物
反応物 4
生成物 1
試薬・触媒・溶媒 1
実験手順
To a solution of 200 mg of 2-amino-1-(3,5-dichloropyridin-2-yl)ethanone-β-ethyloxime and 90 mg of triethylamine in 3 ml of dichloromethane, 169 mg of 2-(trifluoromethyl)benzoyl chloride was added dropwise with stirring under cooling with ice, and after the addition, the mixture was stirred at room temperature for another 30 minutes. After completion of the reaction, the reaction mixture was mixed with 10 ml of water and extracted with ethyl acetate (15 ml×1), the resulting organic layer was washed with water (10 ml×1) and dried over saturated aqueous sodium chloride and then anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography using ethyl acetate-hexane (with a gradient of from 1:9 to 3:7) as the eluent to obtain 190 mg of the desired product as a pale yellow resinous substance.
後処理
- temperatureunder cooling with ice
- additionafter the addition
- stirringthe mixture was stirred at room temperature for another 30 minutes
- customAfter completion of the reaction
- extractionextracted with ethyl acetate (15 ml×1)
- washthe resulting organic layer was washed with water (10 ml×1)
- dry with materialdried over saturated aqueous sodium chloride
- customanhydrous sodium sulfate, and the 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-9054a357c6634b4abced56e566dacb4b
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09434684B2
関連ノート
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