反应详情

36.1 g (133 mmol) of 1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridine-3-carboxamide from Example 3C) are dissolved in 330 ml of THF and treated with 27 g (341 mmol) of pyridine. 47.76 ml (71.66 g, 341 mmol) of trifluoroacetic anhydride are then added in the course of 10 min, the temperature rising to 40° C. The mixture is stirred overnight at room temperature. The batch is then added to 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 hydrogencarbonate solution and with 1 N HCl dried using MgSO4 and concentrated in a rotary evaporator.

1. customrising 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 hydrogencarbonate solution and with 1 N HCl
4. customdried
5. concentrationconcentrated in a rotary evaporator