反应详情

温度

10 °C

To a solution of N-(3-(5-(4-chlorophenyl)-1H-pyrrolo[2,3-b]pyridine-3-carbonyl)-2,4-difluorophenyl)propane-1-sulfonamide (0.2 g, 0.41 mmol) in DMF (1 mL) was added Et3N (165 mg, 1.64 mmol). The reaction was stirred at 10° C. for 10 min, followed by the dropwise addition of a solution of TBAB (264 mg, 1.64 mmol) in DMF (0.5 mL) and a solution of 1-chloroethyl propionate (67 mg, 0.41 mmol) in DMF (0.5 mL) over 30 min. The mixture was stirred at 10° C. for another 3 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 (141 mg, 58%). The title compound was characterized by LCMS and 1H NMR as shown below:

1. stirringThe mixture was stirred at 10° C. for another 3 h
2. filtrationfiltered
3. concentrationThe filtrate was concentrated in vacuo
4. customthe residue was purified by a silica gel column chromatography (PE/EtOAc (v/v)=4/1)