反応式
Br[C:2]1[CH:3]=[C:4]([Cl:28])[C:5]([C:8](=[N:23][O:24][CH:25]([CH3:27])[CH3:26])[CH2:9][NH:10][C:11](=[O:22])[C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=2[C:18]([F:21])([F:20])[F:19])=[N:6][CH:7]=1.[CH3:29][C:30]([CH3:34])([CH3:33])[C:31]#[CH:32].O>C(N(CC)CC)C.[Cu]I>[Cl:28][C:4]1[C:5]([C:8](=[N:23][O:24][CH:25]([CH3:27])[CH3:26])[CH2:9][NH:10][C:11](=[O:22])[C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=2[C:18]([F:21])([F:20])[F:19])=[N:6][CH:7]=[C:2]([C:32]#[C:31][C:30]([CH3:34])([CH3:33])[CH3:29])[CH:3]=1参加物
反応物 3
生成物 1
試薬・触媒・溶媒 2
反応条件
- 温度
- 80 °C
実験手順
To a solution of 0.15 g of N-[2-(5-bromo-3-chloropyridin-2-yl)-2-(isopropoxyimino)ethyl]-2-(trifluoromethyl)benzamide and 0.05 g of 3,3-dimethyl-1-butyne in 3 ml of triethylamine, 0.04 g of copper(I) iodide and 0.02 g of dichlorobistriphenylphosphine palladium(II) were added, and the mixture was stirred at 80° C. for 3 hours. After completion of the reaction, the reaction mixture was allowed to cool to room temperature, mixed with 10 ml of water and extracted with ethyl acetate (20 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 residue was purified by silica gel column chromatography using ethyl acetate-hexane (with a gradient of from 1:5 to 2:4) as the eluent to obtain 0.15 g of the desired product as a yellow resinous substance.
後処理
- customAfter completion of the reaction
- temperatureto cool to room temperature
- extractionextracted with ethyl acetate (20 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 residue was purified by silica gel column chromatography
出典と根拠
- ORDレコード
- ord-18bcfc0220ed4658b8e7553f85be4284
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09434684B2
関連ノート
読み込み中…