反应详情

36.1 g (133 mmol) of 1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridine-3-carboxamide from Example 3A are dissolved in 330 ml of THF, and 27 g (341 mmol) of pyridine are added. Then, over the course of 10 minutes, 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. It 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 bicarbonate solution and with 1N hydrochloric acid, dried with magnesium sulphate 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 1N hydrochloric acid
4. dry with materialdried with magnesium sulphate
5. concentrationconcentrated in a rotary evaporator