HRID230137

反应详情

EQUATION

反应方程式

HRID 230137 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a solution of 2-chloro-5-methylpyridine (10 mL) in 155 mL of glacial acetic acid was added 19 mL of 30% aqueous hydrogen peroxide. The mixture was stirred at 80° C. for 8 hours. The mixture was diluted with 100 mL of water and then concentrated in a vacuum. The residue was made strongly alkaline with anhydrous sodium carbonate and shaken with 200 mL of chloroform. The solids were removed via filtration, and the filtrate was dried over sodium sulfate, filtered and concentrated to give 10.8 g of the 2-chloro-5-methylpyridine-N-oxide (82%). Mass Spec. M+H=144.

WORKUP

后处理

  1. concentrationconcentrated in a vacuum
  2. stirringshaken with 200 mL of chloroform
  3. customThe solids were removed via filtration
  4. dry with materialthe filtrate was dried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated