HRID232159

反应详情

EQUATION

反应方程式

HRID 232159 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a 400 ml flask, 200 ml of o-dichlorobenzene, 1 ml of pyridine and 1.7 g (0.01 mole) of 2-chloro-4-nitroaniline were charged. While stirring the contents at room temperature, 2.5 g (0.01 mole) of 3-trifluoromethylbenzenesulfonylchloride was added gradually over 30 minutes. Thereafter, the reaction mixture was heated and stirred for 8 hours under reflux (175°-180° C.) to complete the reaction. After cooling the reaction mixture to room temperature, it was thoroughly washed first with dilute hydrochloric acid and then with water. Subsequent to its dehydration with sodium sulfate, o-dichlorobenzene was distilled off under reduced pressure. The residue was subjected to silica gel chromatography (eluent: benzene) to isolate the intended Compound 1. m.p. 126°-127° C., yield 1.9 g (50%).

WORKUP

后处理

  1. temperatureThereafter, the reaction mixture was heated
  2. stirringstirred for 8 hours
  3. temperatureunder reflux (175°-180° C.)
  4. customthe reaction
  5. temperatureAfter cooling the reaction mixture to room temperature
  6. washit was thoroughly washed first with dilute hydrochloric acid
  7. distillationSubsequent to its dehydration with sodium sulfate, o-dichlorobenzene was distilled off under reduced pressure