反应详情

温度

100 °C

Ethyl 3-(2,4-difluorophenyl)-1-(4-methoxybenzyl)-1H-thieno[2,3-c]pyrazole-5-carboxylate (1.0103 g, 2.358 mmol) was dissolved in a mixture of 1,2-dichloroethane (11.79 ml) and trifluoroacetic acid (11.79 ml) at 25° C. in a sealed heavy-walled reaction vessel. The reaction mixture was heated to 100° C. and allowed to stir for 2 h. The reaction was stopped, cooled to room temperature, and concentrated under reduced pressure. The residue was taken up in ethyl acetate (20 mL), washed with saturated aqueous sodium bicarbonate (1×15 mL) and saturated aqueous sodium chloride (1×15 mL), dried (sodium sulfate), and concentrated under reduced pressure. The crude product was purified by flash chromatography (RediSep SiO2, 120 g column) on a CombiFlash purification system eluting with ethyl acetate-hexanes (0-60%). The title compound (719.0 mg, 2.332 mmol, 99% yield) was recovered as a white solid. LC-MS [M+1]=309.3.

1. temperaturecooled to room temperature
2. concentrationconcentrated under reduced pressure
3. washwashed with saturated aqueous sodium bicarbonate (1×15 mL) and saturated aqueous sodium chloride (1×15 mL)
4. dry with materialdried (sodium sulfate)
5. concentrationconcentrated under reduced pressure
6. customThe crude product was purified by flash chromatography (RediSep SiO2, 120 g column) on a CombiFlash purification system
7. washeluting with ethyl acetate-hexanes (0-60%)