HRID584676

反应详情

EQUATION

反应方程式

HRID 584676 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
55 °C

PROCEDURE

实验过程

48% aqueous HBr (8.8 M) (3.4 ml, 30 mmol) was slowly added to a stirred solution of 3,4-dichloroacetophenone (1.89 g, 10 mmol) in DMSO (17 ml). The solution was stirred in an open flask at 55° C. for 24 hours. The solution was poured onto ice, the solid product was filtered, washed with water, and redissolved in ethanol (18 ml). 4,5-Dinitro-1,2-phenylene-diamine (890 mg, 4.5 mmol) was added and the mixture was heated to reflux for 4 hours.

WORKUP

后处理

  1. additionThe solution was poured onto ice
  2. filtrationthe solid product was filtered
  3. washwashed with water
  4. dissolutionredissolved in ethanol (18 ml)
  5. temperaturethe mixture was heated
  6. temperatureto reflux for 4 hours