反应详情

HATU (0.061 g, 0.161 mmol) was added to a solution of 3-chloro-5-formyl-1H-pyrrole-2-carboxylic acid (0.028 g, 0.161 mmol), 3-{[3-(aminomethyl)-6-chloro-2-fluorophenyl]oxy}-5-chlorobenzonitrile (0.050 g, 0.161 mmol) and DIPEA (0.028 mL, 0.161 mmol) in DMF (2 mL). The solution was stirred overnight at RT. The reaction mixture was partitioned between water and EtOAc. The organic layer was washed with a 15% Na2CO3 solution and dried over MgSO4. The solid was filtered off and the solvent was evaporated. Purification was accomplished by silica gel column chromatography (EtOAc/hexanes) to give an orange film which was triturated in acetone to afford the title compound (0.012 g, 15%) as a white solid. 1H NMR (400 MHz, DMSO-d6) δ ppm 12.88 (s, 1H), 9.57 (s, 1H), 8.53-8.71 (m, 1H), 7.74-7.86 (m, 1H), 7.47-7.52 (m, 2H), 7.38-7.46 (m, 2H), 7.04 (s, 1H), 4.52 (d, 1H). LCMS: m/z 466.2 (M+1).

1. customThe reaction mixture was partitioned between water and EtOAc
2. washThe organic layer was washed with a 15% Na2CO3 solution
3. dry with materialdried over MgSO4
4. filtrationThe solid was filtered off
5. customthe solvent was evaporated
6. customPurification
7. customto give an orange film which
8. customwas triturated in acetone