反应详情

To a mixture of 3-(2-(4-fluoro-1H-indol-2-yl)-6-(2-(4-fluorophenyl)-3-(methylcarbamoyl)-6-(N-methylmethylsulfonamido)benzofuran-5-yl)pyridin-3-yl)propanoic acid (88 mg, 0.133 mmol) and HATU (126 mg, 0.333 mmol) in DMF (6650 μl) was added DIEA (116 μl, 0.665 mmol). The resultant mixture was stirred for 1 h at ambient temperature then was diluted with EtOAc and washed successively with H2O (3×) and brine (1×). The organic layer was dried over MgSO4, filtered, concentrated in vacuo, and the residue purified by silica gel column chromatography using a gradient of 0-30% EtOAc/CH2Cl2 as eluent. 1H NMR δ (ppm) (CHCl3-d): 8.38 (1H, d, J=8.46 Hz), 8.12 (1H, s), 8.02 (2H, dd, J=8.55, 5.32 Hz), 7.69 (3H, d, J=9.74 Hz), 7.60 (1H, d, J=7.80 Hz), 7.36 (1H, td, J=8.24, 5.56 Hz), 7.25 (2H, t, J=8.60 Hz), 7.02 (1H, t, J=8.68 Hz), 5.95 (1H, br s), 3.35 (3H, s), 3.27˜3.22 (2H, m), 3.20˜3.15 (2H, m), 3.05 (3H, d, J=4.90 Hz), 2.85 (3H, s). MS (M+H)+: 641.

1. washwashed successively with H2O (3×) and brine (1×)
2. dry with materialThe organic layer was dried over MgSO4
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. customthe residue purified by silica gel column chromatography