Potassium Carbonate → HCID 57546030、化合物

HRID 931003

反応式

HRID 931003 の反応式
[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

  1. customThe solvent was evaporated under reduced pressure, to the residue
  2. additionwas added saturated aqueous ammonium chloride solution
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe extract was washed with saturated aqueous ammonium chloride solution and saturated brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. customthe solvent was evaporated under reduced pressure
  7. 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

読み込み中…