HRID1164247

反应详情

EQUATION

反应方程式

HRID 1164247 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Anisil (6.5 g), made by the oxidation of anisoin with copper sulphate in pyridine, was added to acetic acid (50 g) and heated to reflux to form a solution. Hydrobromic acid (s.g. 1.48) was added at reflux until anisil just started to precipitate (about 30 ml HBr being needed). After 2 hours' reflux, more hydrobromic acid (50 ml) was added, and the solution was refluxed for a further 2 hours. After this time, thin layer chromatography showed complete conversion into a single product. The solution was poured into cold water (600 ml) to precipitate a white solid. This was filtered off, washed with water and dried to give 5.5 g of 4,4'-dihydroxybenzil. This was used without further purification.

WORKUP

后处理

  1. temperatureheated
  2. temperatureto reflux
  3. customto form a solution
  4. customto precipitate (about 30 ml HBr being needed)
  5. temperatureAfter 2 hours' reflux
  6. additionmore hydrobromic acid (50 ml) was added
  7. temperaturethe solution was refluxed for a further 2 hours
  8. additionThe solution was poured into cold water (600 ml)
  9. customto precipitate a white solid
  10. filtrationThis was filtered off
  11. washwashed with water
  12. customdried