反应详情

To a solution of 6-(2-(4-fluorophenyl)-3-(methylcarbamoyl)-6-(N-methylmethylsulfonamido)benzofuran-5-yl)-3-methoxypicolinic acid (50 mg, 0.09 mmol), (5-fluoropyridin-2-yl)methanamine (200 mg, 1.58 mmol) and Et3N (0.2 mL) in THF (50 mL) was added T3P (0.05 mL) dropwise at 0° C. and the mixture was stirred for 3 h. After being diluted with water and extracted with EtOAc, the combined organic phases were washed with brine, dried over Na2SO4, filtered and evaporated. The residue was purified by prep-TLC (PE:EtOAc=1:2) to give the pure product of 6-(2-(4-fluorophenyl)-3-(methylcarbamoyl)-6-(N-methylmethylsulfonamido)benzofuran-5-yl)-N-((5-fluoropyridin-2-yl)methyl)-3-methoxypicolinamide (20 mg, yield: 30%). 1H-NMR (CDCl3, 400 MHz) δ 8.60 (t, J=4.8 Hz, 1H), 8.36 (d, J=2.4 Hz, 1H), 7.99 (s, 1H), 7.92˜7.95 (m, 2H), 7.73 (d, J=8.4 Hz, 1H), 7.58 (s, 1H), 7.48 (d, J=8.8 Hz, 1H), 7.24˜7.42 (m, 2H), 7.17˜7.22 (m, 2H), 5.91 (d, J=3.6 Hz, 1H), 4.73 (d, J=5.6 Hz, 2H), 4.01 (s, 3H), 3.18 (s, 3H), 2.97 (d, J=4.8 Hz, 3H), 2.78 (s, 3H). MS (M+H)+: 636.

1. extractionextracted with EtOAc
2. washthe combined organic phases were washed with brine
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. customevaporated
6. customThe residue was purified by prep-TLC (PE:EtOAc=1:2)