反应详情

To a mixture of N-(3-(5-(4-chlorophenyl)-1H-pyrrolo[2,3-b]pyridine-3-carbonyl)-2,4-difluorophenyl)propane-1-sulfonamide (0.1 g, 0.2 mmol), TBAB (132 mg, 0.4 mmol) and Et3N (114 μL, 0.8 mmol) in DMF (1 mL) was added chloromethyl phenyl carbonate (46 mg, 0.25 mmol). The reaction was stirred at rt for 12 h, then diluted with EtOAc (40 mL) and filtered. The filtrate was concentrated in vacuo and the residue was purified by a silica gel column chromatography (PE/EtOAc (v/v)=4/1) to afford the title compound as a white solid (10 mg, 7.7%). The title compound was characterized by LCMS and 1H NMR as shown below:

1. filtrationfiltered
2. concentrationThe filtrate was concentrated in vacuo
3. customthe residue was purified by a silica gel column chromatography (PE/EtOAc (v/v)=4/1)