反应详情

36.1 g (133 mmol) of 1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridine-3-carboxamide from example 1C) are dissolved in 330 ml of THF, and 27 g (341 mmol) of pyridine are added. Then, over the course of 10 min, 47.76 ml (71.66 g, 341 mmol) of trifluoroacetic anhydride are added, during which the temperature rises to 40° C. The mixture is stirred at room temperature overnight. The mixture is then poured into 1 l of water and 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 in a rotary evaporator.

1. customrises to 40° C
2. extractionextracted three times with 0.5 l of ethyl acetate each time
3. washThe organic phase is washed with saturated sodium bicarbonate solution and with 1 N HCl
4. dry with materialdried with MgSO4
5. concentrationconcentrated in a rotary evaporator