反应详情

温度

40 °C

36.1 g (133 mmol) of 1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridine-3-carboxamide from Example 22A are dissolved in 330 ml of THF and mixed with 27 g (341 mmol) of pyridine. Over a period of 10 min, 47.76 ml (71.66 g, 341 mmol) of trifluoroacetic anhydride are subsequently added, and the temperature increases to 40° C. during the addition. The mixture is stirred at room temperature overnight. The mixture is subsequently poured into 1 l of water, and the mixture is extracted three times with 0.5 l of ethyl acetate each time. The organic phase is washed with saturated sodium bicarbonate solution and with 1 N HCl, dried with MgSO4 and concentrated using a rotary evaporator.

1. extractionthe mixture is extracted three times with 0.5 l of ethyl acetate each time
2. washThe organic phase is washed with saturated sodium bicarbonate solution and with 1 N HCl
3. dry with materialdried with MgSO4
4. concentrationconcentrated
5. customa rotary evaporator