Reaktion #1358753

ord-6c098e5333af479e8fa86f557b97bc63

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturunder reflux
  2. 2
    SonstigeThe solvent was evaporated
  3. 3
    Sonstigethe crude residue was purified by flash chromatography (cyclohexane/ethyl acetate 4:1)

Vorschrift

To a solution of Cul (41 mg, 0.2 mmol) in triethylamine (12 ml) were added 2-bromo-4,6-dimethyl-pyridin-3-ylamine (870 mg, 4.33 mmol), (PPh3)2PdCl2 (152 mg, 0.22 mmol), and 1-ethynyl-3-fluorobenzene (500 μl, 4.33 mmol). The reaction mixture was stirred for 30 min. at room temperature and for 3 h under reflux. The solvent was evaporated and the crude residue was purified by flash chromatography (cyclohexane/ethyl acetate 4:1) to yield 745 mg (3.10 mmol, 72%) of (2-(3-fluoro-phenylethynyl)-4,6-dimethyl-pyridin-3-yl)amine as a brown solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07205411B2uspto-grants-2007_04