反应详情

温度

90 °C

In a 100 mL round-bottom flask 6-bromo-3-(trifluoromethyl)-[1,2,4]triazolo[4,3-a]pyridine (2.124 g), 4-trifluoromethoxyphenylboronic acid (2.466 g), and sodium carbonate (0.635 g) were suspended in a mixture of DMF (81 mL) and deionized water (9 mL) that was degassed with nitrogen. Tetrakis(triphenylphosphine) palladium (0.462 g) was added and the reaction mixture stirred at 90° C. overnight, concentrated, the residue dissolved in ethyl acetate, and washed with water (2×) and concentrated NaHCO3. The combined organic phase dried over MgSO4 and concentrated, then subjected to gradient chromatography (ethyl acetate/hexane) to produce dark grey solid. The solid was recrystallized from ethyl acetate/hexanes mixture to produce off-white material.

1. customwas degassed with nitrogen
2. additionTetrakis(triphenylphosphine) palladium (0.462 g) was added
3. concentrationconcentrated
4. dissolutionthe residue dissolved in ethyl acetate
5. washwashed with water (2×) and concentrated NaHCO3
6. dry with materialThe combined organic phase dried over MgSO4
7. concentrationconcentrated
8. customto produce dark grey solid
9. customThe solid was recrystallized from ethyl acetate/hexanes mixture
10. customto produce off-white material