HRID1699930

反应详情

EQUATION

反应方程式

HRID 1699930 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A mixture of 2,7-dimethyl-1H-imidazo[4,5-b]pyridine-4-oxide (4.45 g) in chloroform (4.5 ml) and phosphorous oxychloride (25.4 ml) was stirred at 80° C. for 3 hr and concentrated to dryness under reduced pressure. The residue was poured to ice (75 g), and which was neutralized with aqueous ammonia under ice-cooling. The mixture was stirred at room temperature for 30 min and the precipitated solid was washed with water to give the objective compound (3.66 g) as a gray powder.

WORKUP

后处理

  1. concentrationconcentrated to dryness under reduced pressure
  2. additionThe residue was poured to ice (75 g), and which
  3. temperaturecooling
  4. stirringThe mixture was stirred at room temperature for 30 min
  5. washthe precipitated solid was washed with water