反应详情

温度

100 °C

To a stirring solution of 6-(2-(4-fluorophenyl)-3-(methylcarbamoyl)-6-(N-methylmethylsulfonamido)benzofuran-5-yl)-N-((5-fluoropyridin-2-yl)methyl)-3-methoxypicolinamide (40 mg, 0.05 mmol) in DMF (5 mL) was added Py.HCl (400 mg, 2.22 mmol) under N2 protection. The mixture was stirred in a pre-heated oil-bath at 100° C. for 10 h. The mixture was concentrated in vacuo, diluted with water and extracted with EtOAc. After being washed with brine, dried over Na2SO4, filtered and evaporated, the crude product was purified by prep-TLC (PE:EtOAc=2:1) to give the product of 6-(2-(4-fluorophenyl)-3-(methylcarbamoyl)-6-(N-methylmethylsulfonamido)benzofuran-5-yl)-N-((5-fluoropyridin-2-yl)methyl)-3-hydroxypicolinamide (20 mg, yield: 58%). 1H-NMR (CDCl3, 400 MHz) δ 12.14 (s, 1H), 8.91 (d, J=5.6 Hz, 1H), 8.33 (s, 1H), 7.94 (s, 1H), 7.86˜7.89 (m, 2H), 7.60 (d, J=8.8 Hz, 1H), 7.52 (s, 1H), 7.36 (d, J=8.8 Hz, 1H), 7.31˜7.33 (m, 2H), 7.15 (d, J=8.8 Hz, 2H), 5.78 (d, J=4.0 Hz, 1H), 4.68 (d, J=5.6 Hz, 2H), 3.12 (s, 3H), 2.92 (d, J=4.8 Hz, 3H), 2.76 (s, 3H). MS (M+H)+: 622.

1. concentrationThe mixture was concentrated in vacuo
2. additiondiluted with water
3. extractionextracted with EtOAc
4. washAfter being washed with brine
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. customevaporated
8. customthe crude product was purified by prep-TLC (PE:EtOAc=2:1)