反应详情

温度

60 °C

A solution of Example 171A (30.7 mg, 0.070 mmol) in dioxane (1.0 mL) and distilled water (0.5 mL) was treated with lithium hydroxide monohydrate (9.0 mg, 0.21 mmol), stirred overnight at 60° C., treated with additional lithium hydroxide monohydrate (15.0 mg, 0.357 mmol), heated to 60° C. for an additional three days, and concentrated. The resulting residue was purified by preparative HPLC to provide the desired product. MS (ESI(+)) m/e 425 (M+H)+, 447 (M+Na)+; (ESI(−)) m/e 423 (M−H)−; 1H NMR (300 MHz, DMSO-d6) δ 9.73 (br s, 1H), 8.10 (d, 1H), 7.96 (d, 1H), 7.89 (d, 2H), 7.70 (dt, 1H), 7.54 (m, 5H), 3.49 (t, 2H), 3.04 (t, 2H), 1.86 (q, 2H), 1.70 (t, 2H).

1. temperatureheated to 60° C. for an additional three days
2. concentrationconcentrated
3. customThe resulting residue was purified by preparative HPLC