HRID65609

反应详情

EQUATION

反应方程式

HRID 65609 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 13.81 g. (0.1 mole) of m-nitroaniline in 100 ml. of dry ethyl acetate is added 11.13 g. (0.11 mole) of triethylamine. To the solution is added a solution of 18.56 g. (0.1 mole) of m-nitrobenzoylchloride in 100 ml of ethyl acetate. The mixture is refluxed for 6.5 hours. The reaction mixture is allowed to stand at room temperature overnight. The precipitate is removed by filtration. The filtrate is evaporated to dryness in vacuo. The residue is recrystallized from absolute ethanol. There is obtained 5.79 g. of yellow needles that melt at 188°-189°.

WORKUP

后处理

  1. additionTo the solution is added a solution of 18.56 g
  2. temperatureThe mixture is refluxed for 6.5 hours
  3. customThe precipitate is removed by filtration
  4. customThe filtrate is evaporated to dryness in vacuo
  5. customThe residue is recrystallized from absolute ethanol
  6. customThere is obtained 5.79 g
  7. customthat melt at 188°-189°