HRID2189847
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 25 °C
PROCEDURE
实验过程
To a suspension of (S)—N2-(5-cyclopropyl-1H-pyrazol-3-yl)-N6-[1-(4-fluorophenyl)ethyl]-3-nitropyridine-2,6-diamine (Example 47; 0.26 g, 0.68 mmol) and zinc dust (0.223 g, 3.41 mmol) in MeOH:THF (1:1, 12 ml) was slowly added saturated ammonium chloride solution (1.5 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. Zn dust was removed by filtration and washed with EtOAc (20 ml). The organic layer was separated, washed with brine (10 ml), dried over Na2SO4, and concentrated to give the title compound.
WORKUP
后处理
- stirringThe resulting mixture was stirred for another 30 minutes
- customZn dust was removed by filtration
- washwashed with EtOAc (20 ml)
- customThe organic layer was separated
- washwashed with brine (10 ml)
- dry with materialdried over Na2SO4
- concentrationconcentrated