反应详情

温度

120 °C

To a microwave vial is added [4-(4-bromophenyl)-thiazol-2-yl]-(3-fluorophenyl)-amine (92 mg, 0.26 mmol), 2,2-dimethyl-4-oxo-4-[4-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-phenyl]-butyric acid (half of the crude from last step), sodium carbonate (2M solution, 0.526 mL) and resin bound Pd(PPh3)4 (130 mg, 0.013 mmol). The reaction mixture is sparged with nitrogen for 2 min and then heated in a microwave at 120° C. for 20 min. The resin is then filtered off and the filtrate is concentrated. The residue is titrate with ether. The resulting yellow solid is purified by reverse-phase preparative HPLC to give the title compound: 1H NMR (400 MHz, DMSO-D6) δ ppm 1.24 (s, 6H), 2.49 (d, J=3.54 Hz, 4H), 3.34 (s, 8H), 6.73-6.82 (m, 1H), 7.05 (s, 2H), 7.17 (s, 3H), 7.33 (s, 2H), 7.35-7.40 (m, 2H), 7.50 (s, 1H), 7.81-7.90 (m, 5H), 8.04 (dd, J=8.34, 2.53 Hz, 4H), 10.56 (s, 1H); (M+H)+=475.0.

1. customThe reaction mixture is sparged with nitrogen for 2 min
2. filtrationThe resin is then filtered off
3. concentrationthe filtrate is concentrated
4. customThe resulting yellow solid is purified by reverse-phase preparative HPLC