反应详情

温度

80 °C

To a mixture of N-methyl-2-(4-methyl-2-oxopyridin-1 (2H)-yl)-6-(N-methylmethylsulfonamido)-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzofuran-3-carboxamide (100 mg, 0.19 mmol), 2-chloro-11-fluoro-5,6-dihydroindolo[1,2-h][1,7]naphthyridine (63 mg, 0.23 mmol) and K2CO3 (54 mg, 0.39 mmol) in 1,4-dioxane/H2O (3 mL/0.1 mL) were added X-Phos (10 mg) and Pd2(dba)3 (10 mg) under N2. The reaction mixture was stirred at 80° C. for 5 hours and concentrated in vacuo to remove 1,4-dioxane. The reaction mixture was extracted with EtOAc, washed with brine, dried over Na2SO4, filtered and concentrated in vacuo. The residue was purified by prep-HPLC to give the product (30 mg, yield: 24%). 1H-NMR (CDCl3, 400 MHz) δ 8.17 (s, 1H), 7.83˜7.85 (m, 1H), 7.66˜7.68 (m, 2H), 7.44 (d, J=8.0 Hz, 1H), 7.26˜7.18 (m, 2H), 7.14˜7.18 (m, 2H), 6.77˜6.81 (m, 1H), 6.53 (s, 1H), 6.29 (d, J=8.0 Hz, 1H), 4.34 (t, J=6.4 Hz, 2H), 3.40 (s, 3H), 3.31 (t, J=6.4 Hz, 2H), 2.90 (d, J=4.8 Hz, 3H), 2.61 (s, 3H), 2.32 (s, 3H). MS (M+H)+: 626.

1. concentrationconcentrated in vacuo
2. customto remove 1,4-dioxane
3. extractionThe reaction mixture was extracted with EtOAc
4. washwashed with brine
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. customThe residue was purified by prep-HPLC