反应详情

温度

140 °C

To a solution of 102c (180 mg, 0.468 mol) in dioxane/H2O (12 mL/1 mL) was added 2-(5-fluoro-2-(hydroxymethyl)-3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl)-3,4,6,7,8,9-hexahydropyrazino[1,2-a]indol-1(2H)-one 101l (225 mg, 0.468 mmol), Pd2(dba)3 (43 mg, 0.0468 mmol), tricyclohexylphosphine (131 mg, 0.468 mmol), and Cs2CO3 (305 mg, 0.935 mmol). This mixture was heated in microwave at 140° C. for 1 h. Then, the solid was filtered and the filtrate was concentrated to give a yellow solid, which was further purified by reverse-phase prep-HPLC to afford 102 as a white solid (36 mg, 11%). LCMS: [M+H]+ 663. 1H NMR (500 MHz, DMSO) δ 8.53 (d, J=2.5, 1H), 8.27 (s, 1H), 8.16 (s, 1H), 7.95 (s, 1H), 7.92-7.91 (d, J=2.5, 1H), 7.57 (s, 1H), 7.42-7.36 (m, 2H), 7.36-7.33 (m, 1H), 7.27-7.25 (d, J=9, 1H), 6.53 (s, 1H), 4.88-4.86 (t, J=9, 1H), 4.57-4.54 (m, 2H), 4.47-4.45 (m, 2H), 4.31-4.30 (d, J=4.5, 2H), 4.18-4.13 (m, 3H), 3.92-3.90 (m, 1H), 3.45-3.42 (m, 1H), 3.09-3.10 (m, 4H), 2.64-2.54 (m, 2H), 2.47-2.45 (m, 2H), 2.39-2.38 (m, 4H), 1.79-1.78 (m, 2H), 1.69-1.67 (m, 2H)

1. filtrationThen, the solid was filtered
2. concentrationthe filtrate was concentrated
3. customto give a yellow solid, which
4. customwas further purified by reverse-phase prep-HPLC