HRID703174

反应详情

EQUATION

反应方程式

HRID 703174 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

400 ml of 30% hydrogen peroxide were added dropwise at room temperature to 321.5 g of 2,5-lutidine (2,5-dimethylpyridine) in 1800 ml of glacial acetic acid. The solution was stirred at 80° overnight, then cooled to 40° , treated once more with 400 ml of 30% hydrogen peroxide and heated to 80° for a further 24 hours. After evaporation in vacuo the residue was dissolved in 300 ml of water. The solution was made basic with concentrated sodium hydroxide solution while cooling, saturated with sodium chloride and extracted three times with 1 1 of methylene chloride. The organic extracts were dried over sodium sulfate and evaporated in vacuo. There was obtained 2,5-dimethylpyridine 1-oxide in the form of an oil.

WORKUP

后处理

  1. temperaturecooled to 40°
  2. temperatureheated to 80° for a further 24 hours
  3. customAfter evaporation in vacuo the residue
  4. dissolutionwas dissolved in 300 ml of water
  5. temperaturewhile cooling, saturated with sodium chloride
  6. extractionextracted three times with 1 1 of methylene chloride
  7. dry with materialThe organic extracts were dried over sodium sulfate
  8. customevaporated in vacuo