反应详情

温度

60 °C

To a solution of the title compound from Example 1 Step C (27.0 mg, 0.048 mmol) in 1,4-dioxane (2 mL) was added lithium hydroxide (1.0 mL, 2.0 M aqueous, 2.0 mmol), and the resulting mixture was stirred at 60° C. After 15 min, the reaction mixture was rendered acidic by addition of aqueous hydrochloric acid, then was diluted with 1,4-dioxane and passed through a 0.45 micron syringe filter. Purification by reverse phase HPLC (30 to 100% acetonitrile in water, each with 0.1% v/v TFA) provided the title compound: LCMS m/z 544.4 [M+H]+; 1H NMR (500 MHz, d6-DMSO) δ 8.25 (s, 1H), 8.14-8.07 (m, 2H), 7.74 (d, J=7.5 Hz, 1H), 7.69 (d, J=7.5 Hz, 1H), 7.42 (t, J=7.5 Hz, 1H), 7.32 (d, J=8.0 Hz, 1H), 7.27-7.14 (m, 8H), 7.09 (t, J=8.0 Hz, 1H), 5.19 (s, 2H), 2.86 (app s, 4H).

1. filtrationfilter
2. customPurification by reverse phase HPLC (30 to 100% acetonitrile in water