HRID1761854

反应详情

EQUATION

反应方程式

HRID 1761854 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

At 20° C., with stirring and cooling with ice, a solution of 2,6-dibromo-4-nitro-aniline (47.2 g) in acetic acid (1.6 liters) is slowly poured into a solution of sodium nitrite (12 g) in concentrated sulphuric acid (85 ml). Then, the mixture is stirred for 20 minutes at ambient temperature. The solution thus prepared is then slowly added with stirring and cooling with ice to a solution of copper (I) bromide (12.8 g) in 63% hydrobromic acid (40 ml)/. After it has all been added the mixture is stirred for a further 30 minutes. It is diluted with water, the precipitate is filtered off and washed with water. This crude product is recrystallized from methanol.

WORKUP

后处理

  1. temperaturecooling with ice
  2. stirringThen, the mixture is stirred for 20 minutes at ambient temperature
  3. customThe solution thus prepared
  4. additionis then slowly added
  5. stirringwith stirring
  6. additionall been added the mixture
  7. stirringis stirred for a further 30 minutes
  8. filtrationthe precipitate is filtered off
  9. washwashed with water
  10. customThis crude product is recrystallized from methanol