Potassium Carbonate → 3-Bromo-2-ethynyl-5-(trifluoromethyl)benzenamine

HRID 931003노트

반응식

HRID 931003 반응식
[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]

참가 물질

4

반응물 2

HCID 11430Potassium CarbonateHCID 575462013-Bromo-5-(trifluoromethyl)-2-[(trimethylsilyl)ethynyl]aniline

생성물 1

HCID 575460303-Bromo-2-ethynyl-5-(trifluoromethyl)benzenamine수율 73.6%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-d500e91c93514259ac59da004a617a7a
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09296746B2

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