反应详情

A suspension of Example 93C (1.19 g, 4.9 mmol), 4-fluoro-3-bromobenzonitrile (1.50 g, 7.5 mmol), DMAP (0.12 g, 1 mmol), and potassium carbonate (5.00 g, 36 mmol) in DMSO (13 mL) at room temperature was stirred for 16 hours, quenched with water (20 mL), treated with ethyl acetate (70 mL), and filtered. The filter cake was washed with water and dried at 40° C. under vacuum to provide 1.50 g (72% yield, HPLC purity 95.6%) of the desired product. 1H NMR (400 MHz, DMSO-d6) δ 8.09 (d, 1H), 7.84-7.80 (m, 3H), 7.61-7.58 (m, 3H), 7.37 (d, 1H), 7.16 (d, 1H), 6.56 (br s, 1H), 4.67 (d, 1H), 4.52 (d, 1H), 3.19 (s, 3H).

1. customquenched with water (20 mL)
2. additiontreated with ethyl acetate (70 mL)
3. filtrationfiltered
4. washThe filter cake was washed with water
5. customdried at 40° C. under vacuum