反应详情

温度

100 °C

To a degassed solution of 2-(4-fluorophenyl)-N-methyl-6-(N-methylmethylsulfonamido)-5-(3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl)benzofuran-3-carboxamide (134 mg, 0.27 mmol) and 6-bromo-3-(4-fluorobenzyl)-2H-pyrido[4,3-e][1,3]oxazin-4(3H)-one (75 mg, 0.22 mmol) in DMF (2 mL) were added Pd(dppf)Cl2 (18 mg, 0.02 mmol) and K3PO4 (331 mg, 0.66 mmol) under N2. After being stirred at 100° C. overnight, the reaction mixture was cooled to RT and filtered. The filtrate was washed with brine and dried over Na2SO4. After being concentrated, the residue was purified by prep-TLC (PE:EtOAc=1:1) to give the product of 5-(3-(4-fluorobenzyl)-4-oxo-3,4-dihydro-2H-pyrido[4,3-e][1,3]oxazin-6-yl)-2-(4-fluorophenyl)-N-methyl-6-(N-methylmethylsulfonamido)benzofuran-3-carboxamide (80 mg, yield: 57%). 1H-NMR (CDCl3, 400 MHz) δ 8.52 (s, 1H), 8.08 (s, 1H), 8.01˜7.97 (m, 3H), 7.69 (s, 1H), 7.35 (dd, J=6.0, 8.4 Hz, 2H), 7.20 (t, J=8.4 Hz, 2H), 7.08 (t, J=8.4 Hz, 2H), 5.91 (s, 1H), 5.23 (s, 2H), 4.77 (s, 2H), 3.27 (s, 3H), 3.01 (d, J=4.8 Hz, 3H), 2.85 (s, 3H). MS (M+H)+: 633.

1. temperaturethe reaction mixture was cooled to RT
2. filtrationfiltered
3. washThe filtrate was washed with brine
4. dry with materialdried over Na2SO4
5. concentrationAfter being concentrated
6. customthe residue was purified by prep-TLC (PE:EtOAc=1:1)