反应详情

温度

25 °C

To a suspension of (S)-3-(5-cyclopropyl-1H-pyrazol-3-ylamino)-5-(1-(4-fluorophenyl)ethylamino)-2-nitrobenzonitrile (Method 97; 4.20 g, 10.0 mmol) and zinc dust (3.40 g, 52 mmol) in MeOH-THF (1:1, 100 ml) was slowly added saturated ammonium chloride (40 ml). The reaction mixture was stirred at 25° C. for 1 hour, to which was then added saturated ammonium acetate solution (50 ml). The resulting mixture was stirred for another 30 minutes. Zn dust was removed by filtration and washed with EtOAc (200 ml). The organic layer was separated, washed with brine (100 ml), dried over sodium sulfate, and concentrated. The crude product was used directly for the next step without further purification. MS: Calcd: 394; Found: [M+H]+ 395.

1. stirringThe resulting mixture was stirred for another 30 minutes
2. customZn dust was removed by filtration
3. washwashed with EtOAc (200 ml)
4. customThe organic layer was separated
5. washwashed with brine (100 ml)
6. dry with materialdried over sodium sulfate
7. concentrationconcentrated
8. customThe crude product was used directly for the next step without further purification