HRID1834038

反应详情

EQUATION

反应方程式

HRID 1834038 的结构方程式

PROCEDURE

实验过程

To a stirred solution of 45.12 grams (0.2 moles) of stannous chloride dihydrate in 100 ml. of concentrated HCl is added, gradually, 5.44 grams (0.0282 moles) of 2,4-dinitrobenzonitrile. An exothermic reaction takes place with the temperature rising to about 80°. The solution is stirred and allowed to come to room temperature over the course of 2 hours. The mixture is made strongly basic by the addition of a 50% sodium hydroxide solution, with cooling, and extracted with methylene chloride. The CH2Cl2 extracts are dried over anhydrous MgSO4 and the solvent removed. There is obtained 3.0 grams (80%) of a yellow solid melting at 102°-3°. Infrared (mull): 3500, 3350, (NH), 2200 (CN) cm-1.

WORKUP

后处理

  1. customAn exothermic reaction
  2. customrising to about 80°
  3. customto come to room temperature over the course of 2 hours
  4. temperaturewith cooling
  5. extractionextracted with methylene chloride
  6. dry with materialThe CH2Cl2 extracts are dried over anhydrous MgSO4
  7. customthe solvent removed