HRID1404816

反应详情

EQUATION

反应方程式

HRID 1404816 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 0.8 kg of 4-bromoacetophenone by Sigma-Aldrich Japan, KK., 40 ml of sulfuric acid and 1.2 kg of potassium disulfate was stirred at 180° C. for 18 hours. After stirring, 3.0 L of ethanol was added to the mixture, which was heated to reflux for 7 hours. It was then allowed to naturally cool to room temperature, producing a precipitate which was filtered out. After adding 3.0 L of water to the filtered precipitate and heating to reflux for 1 hour, the reaction mixture was allowed to naturally cool to room temperature. The reaction mixture was filtered and rinsed with 0.5 L of ethanol. In this manner there was obtained 0.58 kg of 1,3,5-tris(p-bromophenyl)benzene.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureto reflux for 7 hours
  3. customproducing a precipitate which
  4. filtrationwas filtered out
  5. additionAfter adding 3.0 L of water to the filtered precipitate
  6. temperatureheating
  7. temperatureto reflux for 1 hour
  8. temperatureto naturally cool to room temperature
  9. filtrationThe reaction mixture was filtered
  10. washrinsed with 0.5 L of ethanol