HRID357554

反应详情

EQUATION

反应方程式

HRID 357554 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

2.0 g (22 mmol) of 3-methoxypropanol was dissolved in 50 ml of dimethyl sulfoxide to obtain a solution. 2.7 g (66 mmol) of sodium hydride was added to this solution at a room temperature. The obtained mixture was stirred at 60° C. for one hour and cooled to a room temperature by allowing to stand, followed by the addition of 3.0 g (19 mmol) of 4-chloro-2,3-dimethylpyridine N-oxide. The obtained mixture was stirred at 40° C. for one hour. After the completion of the reaction, the reaction mixture was distilled to remove the dimethyl sulfoxide. The obtained residue was purified by silica gel column chromatography to obtain 760 mg of 4-(3-methoxypropoxy)-2,3-dimethylpyridine N-oxide.

WORKUP

后处理

  1. customto obtain a solution
  2. temperaturecooled to a room temperature
  3. stirringThe obtained mixture was stirred at 40° C. for one hour
  4. customAfter the completion of the reaction
  5. distillationthe reaction mixture was distilled
  6. customto remove the dimethyl sulfoxide
  7. customThe obtained residue was purified by silica gel column chromatography