HRID595148

反应详情

EQUATION

反应方程式

HRID 595148 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

N-(3-Bromo-5-nitrophenyl)-4-(trifluoromethyl)pyrimidin-2-amine (4.76 g, 13.11 mmol) was dissolved in ethanol (131 ml) and saturated solution of NH4Cl (1 mL) was added followed by Fe (3.66 g, 65.5 mmol). The reaction mixture was stirred at 80° C. for 30 minutes then cooled to room temperature. The solution was filtered through a short pad of silica gel and eluted with EtOAc. The phase were separated, the organics were dried, filtered, concentrated under reduced pressure to afford 5-bromo-N-[4-(trifluoromethyl)pyrimidin-2-yl]benzene-1,3-diamine as a beige powder.

WORKUP

后处理

  1. temperaturethen cooled to room temperature
  2. filtrationThe solution was filtered through a short pad of silica gel
  3. washeluted with EtOAc
  4. customThe phase were separated
  5. customthe organics were dried
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure