HRID728010

反应详情

EQUATION

反应方程式

HRID 728010 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureThe mixture is then refluxed for four hours
  2. customafter which it is evaporated down
  3. washthe solution is washed with water
  4. dry with materialdried with sodium sulfate
  5. customevaporated down
  6. customThe crude product is purified by chromatography over silica gel