反应详情

温度

90 °C

A mixture of Example 3A (5.12 g, 16.9 mmol), Example 2C (3.78 g, 17.9 mmol), Pd2 dba3:CHCl3 (264 mg, 0.255 mmol), xantphos (442 mg, 0.764 mmol), and Cs2CO3 (8.28 g, 25.4 mmol) in dioxane (60 mL) was flushed with N2 and stirred at 90° C. for 16 hours. The mixture was concentrated under reduced pressure, diluted with ethyl acetate, washed sequentially with water and brine, and purified by flash chromatography (0 to 35% ethyl acetate/dichloromethane) to provide the title compound. 1H-NMR (DMSO-d6) δ 8.82 (s, 1H), 8.05 (s, 1H), 7.64 (d, 1H), 7.50-7.53 (m, 3H), 7.20 (t, 1H), 7.14 (d, 1H), 6.81 (t, 1H), 4.45 (d, 2H), 4.00 (s, 3H), 2.70 (ddd, 2H), 1.45 (ddd, 2H), 0.97 (s, 9H).

1. concentrationThe mixture was concentrated under reduced pressure
2. additiondiluted with ethyl acetate
3. washwashed sequentially with water and brine
4. custompurified by flash chromatography (0 to 35% ethyl acetate/dichloromethane)