反应详情

温度

80 °C

To a solution of 5-(11-fluoro-6H-pyrido[2′,3′:5,6][1,3]oxazino[3,4-a]indol-2-yl)-2-(6-methoxypyridin-3-yl)-N-methyl-6-(N-methylmethylsulfonamido)benzofuran-3-carboxamide (40 mg, 0.64 mmol) in HOAc (4 mL) was added HBr—HOAc (4 ml) at 0° C. Then the mixture was stirred at 80° C. for 2 hours. After the solvent was removed by vacuum, the residue was washed with Na2CO3 (a.q.), extracted with DCM, dried over Na2SO4, filtrated and concentrated in vacuo. The residue was purified by prep-HPLC to give the product 5-(11-fluoro-6H-pyrido[2′,3′:5,6][1,3]oxazino[3,4-a]indol-2-yl)-N-methyl-6-(N-methylmethylsulfonamido)-2-(6-oxo-1,6-dihydropyridin-3-yl)benzofuran-3-carboxamide (20 mg, yield: 50%). 1H-NMR (MeOD, 400 MHz) δ 8.33 (s, 1H), 7.96 (q, J=9.6 Hz, 1H), 7.84 (s, 1H), 7.88 (s, 1H), 7.55 (d, J=9.6 Hz, 2H), 7.28 (d, J=9.6 Hz, 1H), 7.15˜7.21 (m, 2H), 6.87 (q, J=9.6 Hz, 1H), 6.53 (t, J=9.6 Hz, 1H), 6.06 (s, 2H), 3.31 (s, 3H), 2.95 (d, J=9.6 Hz, 3H), 2.85 (s, 3H). MS (M+H)+: 614.

1. customAfter the solvent was removed by vacuum
2. washthe residue was washed with Na2CO3 (a.q.)
3. extractionextracted with DCM
4. dry with materialdried over Na2SO4
5. filtrationfiltrated
6. concentrationconcentrated in vacuo
7. customThe residue was purified by prep-HPLC