HRID649695

反应详情

EQUATION

反应方程式

HRID 649695 的结构方程式

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

The temperature is increased to 70° C.-75° C., and a solution is obtained. The solution is held at 70° C.-75° C. for 3 hours. The unreacted bromine is removed by distillation with the aid of 1 liter of carbon tetrachloride. When 1 liter of solvent remains with the product, the solution is cooled to 25° C. The light brown solid which is obtained is filtered and is dried under vacuum for 5 hours. A yield of 250 g (67 percent) is obtained, which analysis by gas chromatography shows to be 97 percent tribromomesitol and 3 percent dibromomesitol. The product has a melting point of 144° C.-146° C. and has the following proton nuclear magnetic resonance spectrum (CDCl3), δ: 2.30 (s, 6H), 4.90 (s, 2H), which is consistent with the structure of the product.

WORKUP

后处理

  1. temperatureThe temperature is increased to 70° C.-75° C.
  2. customa solution is obtained
  3. customThe unreacted bromine is removed by distillation with the aid of 1 liter of carbon tetrachloride
  4. customThe light brown solid which is obtained
  5. filtrationis filtered
  6. customis dried under vacuum for 5 hours
  7. customA yield of 250 g (67 percent) is obtained