反应详情

A mixture of Example 61B (0.05 g, 0.141 mmol), pyridine-3-ylboronic acid (0.018 g, 0.148 mmol) cesium fluoride (0.064 g, 0.423 mmol) and tetrakis(triphenylphosphine)palladium(0) (0.1 g, 0.014 mmol) in DME (2 mL) was heated in a microwave (Personal Chemistry SmithSynthesizer) at 150° C. for 10 minutes. The mixture was filtered evaporated. The residue was purified by HPLC on a C18 column with 0-100% CH3CN/H2O/0.1% TFA to provide the desired product. 1H NMR (400 MHz, DMSO-d6) δ ppm 4.10 (s, 2 H) 5.75 (s, 1 H) 7.41-7.51 (m, 3 H) 7.63-7.73 (m, 2 H) 7.76 (s, 1 H) 7.83-7.88 (m, 1 H) 8.04 (d, J=7.67 Hz, 1 H) 8.12 (dd, J=8.13, 1.38 Hz, 1 H) 8.35 (dt, J=7.98, 1.84 Hz, 1 H) 8.68 (dd, J=5.06, 1.38 Hz, 1 H) 9.01 (d, J=2.15 Hz, 1 H) 12.08 (s, 1 H).

1. filtrationThe mixture was filtered
2. customevaporated
3. customThe residue was purified by HPLC on a C18 column with 0-100% CH3CN/H2O/0.1% TFA