HRID1283785

反应详情

EQUATION

反应方程式

HRID 1283785 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 21 g. of dry pyridine is added slowly with stirring 23 g. (0.26 mol.) of cuprous cyanide. The mixture rapidly solidifies and is then heated to 125°. Excess pyridine is boiled off and the temperature is decreased to 110°. 3-Amino-2-bromobenzotrifluoride (48 g., 0.20 mol.) is added with stirring and the reaction mixture is heated to 165°-170° for 75 minutes. The mixture is then cooled to 90° and a solution of 75 g. (1.05 mol.) of sodium cyanide in 75 ml. of water is added followed by 250 ml. of benzene. The resulting mixture is stirred for one hour, the layers are separated and the benzene layer is washed with water, dried and evaporated to give 2-cyano-3-trifluoromethylaniline.

WORKUP

后处理

  1. temperatureis then heated to 125°
  2. customis decreased to 110°
  3. stirringwith stirring
  4. temperaturethe reaction mixture is heated to 165°-170° for 75 minutes
  5. temperatureThe mixture is then cooled to 90°
  6. stirringThe resulting mixture is stirred for one hour
  7. customthe layers are separated
  8. washthe benzene layer is washed with water
  9. customdried
  10. customevaporated