反应详情

温度

90 °C

To a solution of 5-(4-(4-fluoro-1H-indol-2-yl)-5-vinylpyrimidin-2-yl)-2-(4-fluorophenyl)-N-methyl-6-(N-methylmethylsulfonamido)benzofuran-3-carboxamide (50 mg, 0.08 mmol) in DMAc (1 mL), K3PO4 (100 mg, 0.37 mmol) was added under N2 protection. The reaction mixture was stirred at 90° C. overnight. Then the mixture was diluted with water and extracted with EtOAc. The organic layers were washed with brine, dried over Na2SO4, and concentrated. The residue was purified by prep-HPLC to give the product of 5-(11-fluoro-5,6-dihydropyrimido[4′,5′:3,4]pyrido[1,2-a]indol-2-yl)-2-(4-fluorophenyl)-N-methyl-6-(N-methylmethylsulfonamido)benzofuran-3-carboxamide (10 mg, yield: 20.0%). 1H-NMR (CDCl3, 400 MHz) δ 8.75 (s, 1H), 8.36 (s, 1H), 8.00˜8.10 (m, 2H), 7.75 (s, 1H), 7.53 (s, 1H), 7.15˜7.25 (m, 4H), 6.84 (t, J=8.8 Hz, 1H), 6.01 (br s, 1H), 4.41 (t, J=6.4 Hz, 2H), 3.50 (s, 3H), 3.34 (t, J=6.4 Hz, 2H), 3.05 (d, J=4.8 Hz, 3H), 2.83 (s, 3H). MS (M+H)+: 614

1. extractionextracted with EtOAc
2. washThe organic layers were washed with brine
3. dry with materialdried over Na2SO4
4. concentrationconcentrated
5. customThe residue was purified by prep-HPLC