反应详情

温度

70 °C

A mixture of 2-methyl-2-[5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridin-2-yl]propanenitrile and [6-(1-cyano-1-methylethyl)pyridin-3-yl]boronic acid as trifluoroacetic acid salts (260 mg, approx. 0.673 mmol combined), 5-bromo-2-nitrothiophene-3-carboxamide (169 mg, 0.673 mmol) (Intermediate 10 Step 4), and tetrakis(triphenylphosphine)palladium(0) (38.9 mg, 0.034 mmol) were dissolved in fully degassed tetrahydrofuran (2.7 ml) and fully degassed 2 M aqueous sodium carbonate (0.7 ml). The reaction was stirred at 70° C. for 4 hours. It was then allowed to cool to room temperature, taken up in ethyl acetate, and washed with water (2×) and brine (2×). The organic layer was dried over magnesium sulfate, filtered, and concentrated under reduced pressure. The resulting residue was purified via reverse phase HPLC to yield the title compound.

1. temperatureto cool to room temperature
2. washwashed with water (2×) and brine (2×)
3. dry with materialThe organic layer was dried over magnesium sulfate
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure
6. customThe resulting residue was purified via reverse phase HPLC