反应详情

温度

190 °C

5-Trifluoromethyl-3-trimethylsilanylethynyl-pyridin-2-ylamine (43.8 g, 170 mmol) and copper(I) iodide (6.5 g, 34 mmol) were dissolved in N-methylpyrrolidone (0.85 L). The mixture was stirred at 190° C. for 30 min. The mixture was evaporated to remove N-methylpyrrolidone in vacuo. The residue was purified by flash column chromatography (QingDao silical gel, 200-300 mesh, 40% ethyl acetate/hexanes) to afford 5-trifluoromethyl-1H-pyrrolo[2,3-b]pyridine (7.5 g, 24%) as a yellow solid: LC/MS m/e calcd for C8H5F3N2 [M+H]+ 187.14, observed 187.0.

1. customThe mixture was evaporated
2. customto remove N-methylpyrrolidone in vacuo
3. customThe residue was purified by flash column chromatography (QingDao silical gel, 200-300 mesh, 40% ethyl acetate/hexanes)