HRID1165420

反应详情

EQUATION

反应方程式

HRID 1165420 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 14.3 g of 3-methoxy-6-acetylaminotoluene, 17.8 g of 2-bromo-m-xylene, 6.6 g of potassium carbonate, and 0.3 g of copper (I) iodide was stirred for 42 hours at 160°-210° C. After the reaction mixture was cooled, 22.9 g of potassium hydroxide and 66 ml of n-amyl alcohol were added to the mixture, which was then refluxed for 3.5 hours. Then the reaction mixture was cooled and washed with hot water. The n-amyl alcohol was removed by distillation, and the remaining reaction mixture was distilled under reduced pressure to obtain 5.5 g (28 percent of theoretical yield) of 3-methoxy-6-(2',6'-dimethylanilino)toluene.

WORKUP

后处理

  1. temperatureAfter the reaction mixture was cooled
  2. temperaturewas then refluxed for 3.5 hours
  3. temperatureThen the reaction mixture was cooled
  4. washwashed with hot water
  5. customThe n-amyl alcohol was removed by distillation
  6. customthe remaining reaction mixture
  7. distillationwas distilled under reduced pressure