反应详情

温度

80 °C

Compound A2 (9.52 g, 23.6 mmol) and 2-[3-(2-chloro-3,6-difluoro-phenyl)-isoxazol-5-ylmethoxy]-5-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-pyridine (13.2 g, 29.5 mmol) were dissolved in DME (164 mL), and aq. 2M Na2CO3 (118 mL) was added. The mixture was degassed with N2 (5 min), and Pd(PPh3)4 (1.36 g, 1.18 mmol) was added. The mixture was heated rapidly to 80° C., and was stirred at this temperature for 1 h. The mixture was allowed to cool to rt, and was diluted with EtOAc (200 mL). The mixture was washed with water (200 mL). The org. layer was dried over MgSO4, filtered, and the solvents were removed under reduced pressure. Purification of the crude by FC (heptane→EtOAc/heptane 30:70) yielded the title compound (8.45 g, 62%). LC-MS: tR=1.13 min, ES+: 576.41.

1. additionwas added
2. temperatureto cool to rt
3. washThe mixture was washed with water (200 mL)
4. dry with materiallayer was dried over MgSO4
5. filtrationfiltered
6. customthe solvents were removed under reduced pressure
7. customPurification of the crude by FC (heptane→EtOAc/heptane 30:70)