反应详情

温度

80 °C

To a degassed solution of 2-(4-fluorophenyl)-N-methyl-6-(N-methylmethylsulfonamido)-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzofuran-3-carboxamide (110 mg, 0.22 mmol), 2-chloro-7-fluoro-6-(thiophen-2-yl)-6,11-dihydropyrido[2′,3′:5,6]pyrano[4,3-b]indole (78 mg, 0.22 mmol) and K3PO4 (176 mg, 0.66 mmol) in dioxane/H2O (0.8 mL/0.2 mL) was added Pd2(dba)3 (10 mg, 0.011 mmol) and X-Phos (10 mg, 0.022 mmol) under N2. The mixture was heated to 80° C. and then stirred for 1 hour. The reaction mixture was cooled to RT, diluted with EtOAc and filtered. The filtrate was washed with H2O, brine, dried over Na2SO4. After concentrated, the resulting residue was purified using Prep-TLC (petroleum ether:EtOAc=1:1) to provide the desired product of compound 66 (65 mg, yield 42.7%). 1H-NMR (CDCl3, 400 MHz) δ 9.94 (s, 1H), 7.96 (s, 1H), 7.89˜7.91 (m, 2H), 7.51 (s, 1H), 7.04˜7.34 (m, 8H), 6.91 (s, 1H), 6.85 (t, J=4.0 Hz, 1H), 6.68 (t, J=9.2 Hz, 1H), 5.81 (br s, J=3.6 Hz, 1H), 3.02 (s, 3H), 2.93 (s, 6H). MS (M+H)+: 697.

1. temperatureThe reaction mixture was cooled to RT
2. filtrationfiltered
3. washThe filtrate was washed with H2O, brine
4. dry with materialdried over Na2SO4
5. concentrationAfter concentrated
6. customthe resulting residue was purified