反应详情

温度

-20 °C

48% HBr 50 mL was added to 6.9 g (40 mmol) of 2-amino-6-phenylpyridine and stirred. The solution was cooled down to −20° C., and 7.7 g (48 mmol) of bromine was dropwise added thereto. Further, 2.8 g (40 mmol) of sodium nitrite was dropwise added thereto. The solution was stirred for 3 hours while elevating the temperature up to room temperature. After finishing the reaction, the solution was extracted with ethyl acetate, and the aqueous layer was removed. The organic layer was dried on anhydrous magnesium sulfate, and the solvent was removed by distillation under reduced pressure. The residue was refined by silica gel chromatography to obtain 7.5 g (yield: 80%) of 2-bromo-6-phenylpyridine.

1. stirringThe solution was stirred for 3 hours
2. customup to room temperature
3. customthe reaction
4. extractionthe solution was extracted with ethyl acetate
5. customthe aqueous layer was removed
6. dry with materialThe organic layer was dried on anhydrous magnesium sulfate
7. customthe solvent was removed by distillation under reduced pressure