反应详情

温度

80 °C

A 100 mL, round-bottomed flask was charged with 6-chloro-2-fluoro-N-(3-methoxy-1-(4-methoxybenzyl)-1H-pyrazolo[3,4-b]pyridin-5-yl)-3-(3-(4-methoxyphenoxy)propylsulfonamido)benzamide (228.3 mg, 0.33 mmol) and TFA (0.5 mL). The reaction mixture was stirred at 80° C. until LC-MS showed that the starting material had been consumed (overnight). Then the CF3COOH was removed under reduced pressure. The residue was purified by silica gel chromatography (EtOAc/hexane from 1/4 to 1/0, v/v) to afford 6-chloro-2-fluoro-N-(3-methoxy-1H-pyrazolo[3,4-b]pyridin-5-yl)-3-(3-(4-methoxyphenoxy)propylsulfonamido)benzamide (181.4 mg, 96.38%). LRMS (APCI pos): >95% purity, 254 nm, m/e 564.1 and 566.1 (M+1).

1. customhad been consumed (overnight)
2. customThen the CF3COOH was removed under reduced pressure
3. customThe residue was purified by silica gel chromatography (EtOAc/hexane from 1/4 to 1/0