反应详情

A mixture of 2-fluoropyridin-3-amine (44.6 mmol) and KOAc (44.6 mmol) in AcOH was stirred at room temperature for 1 h. The mixture was cooled to 0 C and Br2 (44.6 mmol) was added dropwise. The mixture was stirred at 0° C. for 15 min. The mixture was concentrated and the residue was dissolved in EtOAc/MeOH. The organic solution was washed (sat. NaHCO3, sat. Na2S2O3), dried (Na2SO4) and concentrated. The residue was purified by flash column chromatography (SiO2, 100:0 to 80:20 petroleum ether/EtOAc) to yield the desired product.

1. additionwas added dropwise
2. stirringThe mixture was stirred at 0° C. for 15 min
3. concentrationThe mixture was concentrated
4. dissolutionthe residue was dissolved in EtOAc/MeOH
5. washThe organic solution was washed (sat. NaHCO3, sat. Na2S2O3)
6. dry with materialdried (Na2SO4)
7. concentrationconcentrated
8. customThe residue was purified by flash column chromatography (SiO2, 100:0 to 80:20 petroleum ether/EtOAc)