HRID1092230

反应详情

EQUATION

反应方程式

HRID 1092230 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

To a suspension of (S)-N1-(5-cyclopropyl-1H-pyrazol-3-yl)-4-fluoro-N3-[1-(4-fluorophenyl)ethyl]-6-nitrobenzene-1,3-diamine (Method 38; 0.33 g, 0.826 mmol) and Zinc dust (0.270 g, 4.13 mmol) in MeOH:THF (1:1, 10 ml) was slowly added saturated ammonium chloride (4 ml). The mixture was stirred at 25° C. for 2 hrs, to which was added saturated ammonium acetate solution (5 ml). The resulting mixture was stirred for another 30 min. The Zn dust was removed by filtration and washed with EtOAc (15 ml). The organic layer was separated and dried over Na2SO4. After removal of solvent, the title compound was used directly for the next step without further purification.

WORKUP

后处理

  1. stirringThe resulting mixture was stirred for another 30 min
  2. customThe Zn dust was removed by filtration
  3. washwashed with EtOAc (15 ml)
  4. customThe organic layer was separated
  5. dry with materialdried over Na2SO4
  6. customAfter removal of solvent
  7. customthe title compound was used directly for the next step without further purification