反应详情

温度

100 °C

A mixture of 5-(4-(4-fluoro-1H-indol-2-yl)-5-(2-methylprop-1-en-1-yl)pyridin-2-yl)-2-(4-fluorophenyl)-N-methyl-6-(N-methylmethylsulfonamido)benzofuran-3-carboxamide (100 mg, 0.156 mmol) and K3PO4 (166 mg, 0.781 mmol) in DMAc (0.8 mL) was stirred at 100° C. overnight. The mixture was then diluted with water (40 mL) and extracted with EA (20 mL*3). The organic layer was washed with brine (30 mL*3), dried over Na2SO4 and concentrated. The residue was purified by prep-TLC (DCM:EA=1:1) to afford the product of 5-(11-fluoro-6,6-dimethyl-5,6-dihydroindolo[2,1-a][2,6]naphthyridin-2-yl)-2-(4-fluorophenyl)-N-methyl-6-(N-methylmethylsulfonamido)benzofuran-3-carboxamide (40 mg, yield: 40.0%). 1H-NMR (CDCl3, 400 MHz) δ 8.49 (s, 1H), 7.86˜8.00 (m, 4H), 7.61 (s, 1H), 7.45 (d, J=8.0 Hz, 1H), 7.00˜7.18 (m, 4H), 6.72 (t, J=8.4 Hz, 1H), 6.01 (br s, 1H), 3.16 (s, 3H), 3.08 (br s, 2H), 2.93 (d, J=4.4 Hz, 3H), 2.77 (s, 3H), 1.69 (br s, 6H). MS (M+H)+: 641.

1. extractionextracted with EA (20 mL*3)
2. washThe organic layer was washed with brine (30 mL*3)
3. dry with materialdried over Na2SO4
4. concentrationconcentrated
5. customThe residue was purified by prep-TLC (DCM:EA=1:1)