反応式
[Br:1][C:2]1[C:3]([C:13]#[C:14][Si](C)(C)C)=[C:4]([CH:6]=[C:7]([C:9]([F:12])([F:11])[F:10])[CH:8]=1)[NH2:5].C(=O)([O-])[O-].[K+].[K+]>CO>[Br:1][C:2]1[C:3]([C:13]#[CH:14])=[C:4]([CH:6]=[C:7]([C:9]([F:10])([F:11])[F:12])[CH:8]=1)[NH2:5]参加物
4
実験手順
To a solution of 3-bromo-5-(trifluoromethyl)-2-((trimethylsilyl)ethynyl)aniline (2.70 g) in methanol (30 mL) was added potassium carbonate (1.11 g), and the mixture was stirred overnight at room temperature. The solvent was evaporated under reduced pressure, to the residue was added saturated aqueous ammonium chloride solution, and the mixture was extracted with ethyl acetate. The extract was washed with saturated aqueous ammonium chloride solution and saturated brine, and dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (1.56 g).
後処理
- customThe solvent was evaporated under reduced pressure, to the residue
- additionwas added saturated aqueous ammonium chloride solution
- extractionthe mixture was extracted with ethyl acetate
- washThe extract was washed with saturated aqueous ammonium chloride solution and saturated brine
- dry with materialdried over anhydrous sodium sulfate
- customthe solvent was evaporated under reduced pressure
- customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane)
出典と根拠
- ORDレコード
- ord-d500e91c93514259ac59da004a617a7a
- 出典データセット
- uspto-grants-2016_03
- 特許番号
- US09296746B2
関連ノート
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