反应详情

To a solution of 3-(benzyloxy)-N-(4-fluorobenzyl)-6-(2-(4-fluorophenyl)-3-(methylcarbamoyl)-6-(N-methylmethylsulfonamido)benzofuran-5-yl)picolinamide (361 mg, 0.51 mmol) in CH3OH (5 mL) was added Pd—C under Ar. The suspension was degassed under vacuum and purged with H2 several times. The mixture was stirred under H2 at RT overnight. After being filtered through celite and removal of the solvent by concentration, the residue was purified by prep-TLC (DCM:MeOH=60:1) to afford the product of N-(4-fluorobenzyl)-6-(2-(4-fluorophenyl)-3-(methylcarbamoyl)-6-(N-methylmethylsulfonamido)benzofuran-5-yl)-3-hydroxypicolinamide. (220 mg, yield: 70%). 1H-NMR (CDCl3, 400 MHz) δ 12.27 (s, 1H), 8.61˜8.64 (m, 1H), 7.91˜7.96 (m, 3H), 7.64 (d, J=8.8 Hz, 1H), 7.55 (s, 1H), 7.42 (d, J=8.4 Hz, 1H), 7.35 (dd, J=5.6, 8.4 Hz, 2H), 7.21 (t, J=8.4 Hz, 2H), 7.01 (t, J=8.4 Hz, 2H), 5.80 (d, J=3.6 Hz, 1H), 4.59 (d, J=6.4 Hz, 2H), 3.04 (s, 3H), 2.97 (d, J=5.2 Hz, 3H), 2.91 (s, 3H). MS (M+H)+: 621.

1. customThe suspension was degassed under vacuum
2. custompurged with H2 several times
3. filtrationAfter being filtered through celite and removal of the solvent by concentration
4. customthe residue was purified by prep-TLC (DCM:MeOH=60:1)