反应详情

温度

150 °C

Under an atmosphere of argon, 6.370 g (purity 83%, 15.447 mmol) of 1-(cyclopentylmethyl)-5-fluoro-3-iodo-1H-pyrazolo[3,4-b]pyridine and 1.522 g (16.992 mmol) of copper(I) cyanide were initially charged in 45 ml of absolute DMSO, and the mixture was heated at 150° C. for 1.5 h. After cooling, the reaction was diluted with methanol and filtered through Celite. The organic phase was washed twice with a mixture of 25% strength aqueous ammonia solution and saturated aqueous ammonium chloride solution (v/v=1:3), then washed with a saturated aqueous sodium chloride solution, dried over sodium sulfate and concentrated on a rotary evaporator. This gave 3.670 g (purity 86%, 97% of theory) of the target compound.

1. temperatureAfter cooling
2. filtrationfiltered through Celite
3. washThe organic phase was washed twice with a mixture of 25% strength aqueous ammonia solution and saturated aqueous ammonium chloride solution (v/v=1:3)
4. washwashed with a saturated aqueous sodium chloride solution
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated on a rotary evaporator