HRID631785

反应详情

EQUATION

反应方程式

HRID 631785 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

8-hydroxy-2-methylquinoline (2 g, 12.4 mmol.), selenium dioxide (1.74 g, 15.8 mmol), 300 ml of pre-dried 1,4-dioxane, and 1.5 ml of water were mixed and stirred in a 1-L round bottom flask. The resulting solution was then refluxed for 24 h. The reaction was monitored until completion using TLC method. The reaction mixture was then filtered off, and the selenium metal was then washed with dichloromethane, and the combined filtrates were then evaporated off under reduced pressure. The crude product was then purified by sublimation under reduced pressure or by silica gel column chromatography to yield pure yellow needle crystal.

WORKUP

后处理

  1. temperatureThe resulting solution was then refluxed for 24 h
  2. filtrationThe reaction mixture was then filtered off
  3. washthe selenium metal was then washed with dichloromethane
  4. customthe combined filtrates were then evaporated off under reduced pressure
  5. customThe crude product was then purified by sublimation under reduced pressure or by silica gel column chromatography
  6. customto yield pure yellow needle crystal