反应详情

2,5-Dibromopyridine (12.6 g, 53.0 mmol) and [3-(2-chloro-3,6-difluoro-phenyl)-isoxazol-5-yl]-methanol (10.0 g, 40.7 mmol) were dissolved in toluene (400 mL). tBuONa (5.87 g, 61.1 mmol), xantphos (1.42 g, 2.45 mmol) and Pd2(dba)3 (732 mg, 0.800 mmol) were added to the sol. The resulting mixture was refluxed overnight, and was allowed to cool down to rt. The mixture was filtered through Celite (washed with EtOAc), and was washed with aq. sat. NaHCO3 (1×) and brine (2×). The org. layer was dried over MgSO4, filtered, and concentrated under reduced pressure. Purification of the crude by FC (EtOAc/heptane 10:90) yielded the title compound (10.6 g, 65%). LC-MS: tR=1.10 min; ES+: 400.66.

1. temperaturewas refluxed overnight
2. filtrationThe mixture was filtered through Celite (washed with EtOAc)
3. washwas washed with aq. sat. NaHCO3 (1×) and brine (2×)
4. dry with materiallayer was dried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customPurification of the crude by FC (EtOAc/heptane 10:90)