HRID728010
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
21.4 g (0.133 mol) of bromine are added, while stirring, to 27.5 g (0.133 mol) of 2-methylphenylglyoxylic acid methyl ester O-methyloxime dissolved in 400 ml of tetrachloromethane. The mixture is then refluxed for four hours while being exposed to a 300 W Hg vapor lamp, after which it is evaporated down, the residue is taken up in ethyl acetate/water and the solution is washed with water, dried with sodium sulfate and evaporated down. The crude product is purified by chromatography over silica gel, using 9:1 cyclohexane/ethyl acetate. 17.4 g (46%) of the abovementioned compound are obtained as an oil.
WORKUP
后处理
- temperatureThe mixture is then refluxed for four hours
- customafter which it is evaporated down
- washthe solution is washed with water
- dry with materialdried with sodium sulfate
- customevaporated down
- customThe crude product is purified by chromatography over silica gel