反应详情

温度

25 °C

To a suspension of (R)-2-(4-(5-cyclopropyl-1H-pyrazol-3-ylamino)-5-nitropyridin-2-ylamino)-2-(4-fluorophenyl)ethanol (Method 94, 0.14 g, 0.36 mmol) and zinc dust (0.12 g, 1.78 mmol) in MeOH-THF (1:1, 16 ml) was slowly added saturated ammonium chloride (2.0 ml). The reaction mixture was stirred at 25° C. for 1 hour, to which was then added saturated ammonium acetate solution (5 ml). The resulting mixture was stirred for another 30 minutes. The Zn dust was removed by filtration and washed with EtOAc (20 ml). The organic layer was separated, washed with brine (10 ml), dried over sodium sulfate, and concentrated. The crude product was used directly for the next step without further purification. MS: Calcd.: 368; Found: [M+H]+ 369.

1. stirringThe resulting mixture was stirred for another 30 minutes
2. customThe Zn dust was removed by filtration
3. washwashed with EtOAc (20 ml)
4. customThe organic layer was separated
5. washwashed with brine (10 ml)
6. dry with materialdried over sodium sulfate
7. concentrationconcentrated
8. customThe crude product was used directly for the next step without further purification