反应详情

温度

-78 °C

In a three neck round bottle flask, to a mixture of 1,3-difluorobenzene (23.24 mmol, 2.29 ml) in THF (30 ml) at −78° C. under argon atmosphere, a solution of n-BuLi (10.2 ml) in THF (2.5M) was added. The mixture was stirred at −78° C. for 30 minutes and then it was heated to −50° C. A solution of ZnCl2 (51 ml) in THF (0.5M) was added drop wise and the mixture was stirred at this temperature for 20 minutes. A solution of 6-bromopyridin-3-amine (11.56 mmol, 2.0 g) in THF (20 ml) and Pd(PPh3)4 (1.16 mmol, 1.3 g) were added respectively and the crude mixture was heated at 40° C. overnight. The solvent was evaporated and the crude mixture was purified by reverse phase chromatography eluting with a water-MeOH/AcN system affording 0.72 g (yield 30%) of the expected product.

1. temperatureit was heated to −50° C
2. stirringthe mixture was stirred at this temperature for 20 minutes
3. customThe solvent was evaporated
4. customthe crude mixture was purified by reverse phase chromatography
5. washeluting with a water-MeOH/AcN system