Potassium Carbonate → HCID 57546030, Verbindung

HRID 931003

Reaktionsgleichung

Reaktionsgleichung von HRID 931003
[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]

Komponenten

4

Edukt 2

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

Produkt 1

HCID 57546030HCID 57546030, VerbindungAusbeute 73,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

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).

Aufarbeitung

  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)

Quellen und Nachweise

ORD-Eintrag
ord-d500e91c93514259ac59da004a617a7a
Quelldatensatz
uspto-grants-2016_03
Patentnummer
US09296746B2

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