反应详情

温度

100 °C

Example 3 was prepared according to the general procedure of Example 2. Intermediate 2A (0.32 mmol), potassium carbonate (140 mg, 1.01 mmol), 4-methylpyrimidin-5-ylboronic acid hydrochloride salt (78 mg, 0.45 mmol), NMP (1.0 mL), PdCl2(dppf).CH2Cl2 (45 mg, 0.056 mmol), and deoxygenated water (50 μL) were heated at 100° C. for 4 h to give 37.5 mg (63%) of the title compound as an off white solid. Purification was done by preparative HPLC (Condition A) using a Phenomenex Luna Axia 30×100 mm S10 column from 15% Solvent B to 85% Solvent B over 12 min, ret. T=9.3 min. 1H NMR (500 MHz, MeOD) δ ppm 2.36 (s, 3 H) 7.29-7.35 (m, 3 H) 7.54 (d, J=5.19 Hz, 1 H) 8.10 (s, 1 H) 8.26-8.32 (m, 2 H) 8.55 (s, 1 H) 8.57 (d, J=5.19 Hz, 1 H) 8.74 (d, J=4.58 Hz, 1 H). LC/MS (Condition B): ret. T=1.82 min, (M+H)+ 305.09. Analytical HPLC: (Condition A): >99%, ret. T=23.46 min, (Condition B): >99%, ret. T=23.49 min, (Condition C): >98%, ret. T=10.4 min, (Condition D): >98%, ret. T=10.6 min.

1. customExample 3 was prepared