反应详情

温度

90 °C

A mixture of the title compound from Example 300 Step A (50.0 mg, 0.086 mmol), 4-trifluoromethylphenylboronic acid (35 mg, 0.18 mmol), trans-dichlorobis(triphenylphosphine) palladium (II) (9.0 mg, 0.013 mmol), Na2CO3 (0.1 mL, 2.0 M aqueous, 0.2 mmol), and MeCN (1 mL) was stirred at 90° C. for 35 min. The crude mixture was dried concentrated in vacuo. Treatment with a mixture of 0.1 mL each of 3 N NaOH, dioxane and MeOH at 50° C. for 10 min, followed by reverse phase HPLC using a YMC C-18 column (65 to 100% acetonitrile in water, each with 0.1% v/v TFA) provided the title compound: LCMS m/z 599.9 [M−F]+; 1H NMR (500 MHz, acetone-d6) δ 8.34 (m, 2H), 8.03 (d, J=7.6 Hz, 1H), 7.99 (d, J=8.2 Hz, 1H), 7.95-7.78 (m, 7H), 7.69 (d, J=8.5 Hz, 2H), 7.62 (m, 2H).

1. dry with materialThe crude mixture was dried
2. concentrationconcentrated in vacuo
3. additionTreatment with a mixture of 0.1 mL each of 3 N NaOH, dioxane and MeOH at 50° C. for 10 min