反应详情

温度

80 °C

To a suspension of 4-bromopyridine hydrochloride (3.9 g, 20 mmol), tetrakis(triphenylphosphine)palladium (2.32 g, 2.0 mmol), triethylamine (16.8 mL, 120 mmol) in dry DMF (150 mL) is added phenylacetylene (4.2 mL, 40 mmol) at room temperature. After stirring for 3 hours at 80° C., the reaction mixture is concentrated. The residue is dissolved in CH2Cl2 (100 mL), washed with H2O, brine (50 mL), dried (MgSO4) and concentrated. The crude material is purified by chromatography (silica gel, EtOAc/hexane: 10/90) to afford the title compound as a solid (3.25 g, 91%). Mp 51-53° C. MS (+) ES: 180 (M+H)+.

1. concentrationthe reaction mixture is concentrated
2. dissolutionThe residue is dissolved in CH2Cl2 (100 mL)
3. washwashed with H2O, brine (50 mL)
4. dry with materialdried (MgSO4)
5. concentrationconcentrated
6. customThe crude material is purified by chromatography (silica gel, EtOAc/hexane: 10/90)