HRID463796

反应详情

EQUATION

反应方程式

HRID 463796 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To a mixed solution of 150 g of stannous chloride and 200 ml of concentrated sulfuric acid under ice-cooling is added 29 g of 2-chloro-6-nitrotoluene. Then, the solution is heated at 100° C. for 1 hour, resulting in white crystals. The crystals are recovered by filtration and dissolved in a mixed solution of 400 ml of water and 50 ml of a 40% NaOH solution, followed by extracting with 500 ml of chloroform. After washing the extract with 400 ml of water, the chloroform layer is dried over anhydrous magnesium sulfate, and the solvent is distilled off under reduced pressure for concentration. Distillation of the resultant residue yields 23 g of 2-methyl-3-chloroaniline as the fraction of 115°-116° C./10 mmHg.

WORKUP

后处理

  1. customresulting in white crystals
  2. filtrationThe crystals are recovered by filtration
  3. dissolutiondissolved in a mixed solution of 400 ml of water and 50 ml of a 40% NaOH solution
  4. extractionby extracting with 500 ml of chloroform
  5. washAfter washing the
  6. extractionextract with 400 ml of water
  7. dry with materialthe chloroform layer is dried over anhydrous magnesium sulfate
  8. distillationthe solvent is distilled off under reduced pressure for concentration
  9. distillationDistillation of the resultant residue