HRID446999

反应详情

EQUATION

反应方程式

HRID 446999 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

To an ice-cold solution of 2,6-dibromo-4-nitro-aniline (100 g, 0.34 mol) in 1.50 L of ethanol was added dropwise conc. H2SO4 (116 ml, 2.15 mol) over 30-45 min with constant stirring. The reaction mixture was heated to 60° C. and sodium nitrite (72 g, 1.09 mol) was added to the reaction mixture portion wise. The resulting yellow colored reaction mixture was heated slowly to 90° C. and refluxed for 2 to 2.5 h. After cooling to room temperature, the mixture was poured into ice water. The reddish brown solid thus obtained was filtered, washed with water and dried to give the desired compound as a brown solid (85.0 g, 90%).

WORKUP

后处理

  1. temperatureThe resulting yellow colored reaction mixture was heated slowly to 90° C.
  2. temperaturerefluxed for 2 to 2.5 h
  3. temperatureAfter cooling to room temperature
  4. customThe reddish brown solid thus obtained
  5. filtrationwas filtered
  6. washwashed with water
  7. customdried