反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureheated
- temperatureto reflux
- customto form a solution
- customto precipitate (about 30 ml HBr being needed)
- temperatureAfter 2 hours' reflux
- additionmore hydrobromic acid (50 ml) was added
- temperaturethe solution was refluxed for a further 2 hours
- additionThe solution was poured into cold water (600 ml)
- customto precipitate a white solid
- filtrationThis was filtered off
- washwashed with water
- customdried