反应详情

温度

150 °C

A suspension of 16.03 g (43.19 mmol) of 5-fluoro-1-(2-fluorobenzyl)-3-iodo-1H-pyrazolo[3,4-b]pyridine (Example 7A) and 4.25 g (47.51 mmol) of copper cyanide was initially charged in DMSO (120 ml) and stirred at 150° C. for 2 h. After cooling, the contents of the flask were cooled to about 40° C., poured into a solution of conc. ammonia water (90 ml) and water (500 ml), ethyl acetate (200 ml) was added and the mixture was stirred briefly. The aqueous phase was separated off and extracted two more times with ethyl acetate (200 ml each). The combined organic phases were washed twice with 10% strength aqueous sodium chloride solution (100 ml each), dried and concentrated under reduced pressure. The crude product was reacted without further purification.

1. temperatureAfter cooling
2. temperaturethe contents of the flask were cooled to about 40° C.
3. additionwas added
4. stirringthe mixture was stirred briefly
5. customThe aqueous phase was separated off
6. extractionextracted two more times with ethyl acetate (200 ml each)
7. washThe combined organic phases were washed twice with 10% strength aqueous sodium chloride solution (100 ml each)
8. customdried
9. concentrationconcentrated under reduced pressure
10. customThe crude product was reacted without further purification