反应详情

温度

25 °C

A solution of saturated ammonium chloride (3 ml) was added slowly to a suspension of (R)-2-(4-fluorophenyl)-2-(6-(5-methyl-1H-pyrazol-3-ylamino)-3-nitropyridin-2-ylamino)ethanol (Method 63, 0.29 g, 0.78 mmol) and zinc dust (0.25 g, 3.9 mmol) in a mixture of MeOH-THF (1:1, 20 ml). The mixture was stirred at 25° C. for 1 hour. Saturated ammonium acetate solution (5 ml) was added and the mixture was stirred for another 30 minutes. The Zn dust was removed by filtration and the cake was washed with EtOAc (20 ml). The organic layer was separated, washed with brine (10 ml) and dried over sodium sulfate. After removal of solvent, the title compound was obtained which was used directly for the next step without purification. MS: Calcd.: 342. Found: [M+H]+ 343.

1. stirringthe mixture was stirred for another 30 minutes
2. customThe Zn dust was removed by filtration
3. washthe cake was washed with EtOAc (20 ml)
4. customThe organic layer was separated
5. washwashed with brine (10 ml)
6. dry with materialdried over sodium sulfate
7. customAfter removal of solvent