反应详情

温度

120 °C

5-Bromo-1H-indole [CA.S. 10075-50-0] (2 g, 10.202 mmol) was dissolved in DMF (16 ml). A nitrogen stream was bubbled through the mixture and then were added 3-Fluoro-4-iodopyridine [CA.S. 22282-75-3] (2.502 g, 11.222 mmol), lithium chloride (0.432 g, 10.202 mmol), copper(I) iodide (0.0195 g, 0.102 mmol) and K2CO3 (4.23 g, 30.605 mmol). The reaction mixture was heated at 120° C. for 2 days. After cooling to room temperature, the reaction mixture was refilled with lithium chloride (0.100 g) and (copper(I) iodide (0.010) stirred at 120° C. for 16 h. After cooling to room temperature, the reaction mixture was washed with NH3 (aqueous sat. solution) and extracted with DCM. The organic layer was separated, washed with water, dried (Na2SO4), and the solvent was evaporated in vacuo. The residue was purified by column chromatography (silica gel; eluent:Heptane/EtOAc up to 15% as eluent). The desired fractions were collected and the solvent was evaporated in vacuo to yield intermediate compound D20 (1.37 g, 46%).

1. customA nitrogen stream was bubbled through the mixture
2. temperatureAfter cooling to room temperature
3. temperatureAfter cooling to room temperature
4. washthe reaction mixture was washed with NH3 (aqueous sat. solution)
5. extractionextracted with DCM
6. customThe organic layer was separated
7. washwashed with water
8. dry with materialdried (Na2SO4)
9. customthe solvent was evaporated in vacuo
10. customThe residue was purified by column chromatography (silica gel; eluent:Heptane/EtOAc up to 15% as eluent)
11. customThe desired fractions were collected
12. customthe solvent was evaporated in vacuo
13. customto yield intermediate compound D20 (1.37 g, 46%)