HRID1955004

反应详情

EQUATION

反应方程式

HRID 1955004 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A suspension of 3-chloro-2-methyl-8-pivaloylaminoimidazo[1,2-a]pyridine (4.0 g, 15 mmol) in 60% strength sulfuric acid (25 ml) is stirred at 100° C. for 1 h. After cooling to RT, water (100 ml) is added and the mixture is adjusted to pH 10 using 10 N sodium hydroxide solution. It is then extracted with ethyl acetate (3×50 ml). The combined organic extracts are washed with water (50 ml), dried over magnesium sulfate and concentrated. The residue is taken up in boiling toluene, clarified with silica gel and crystallized. The title compound is isolated as a beige solid. Yield 1.9 g (70%), m.p. 126-127° C.

WORKUP

后处理

  1. temperatureAfter cooling to RT
  2. extractionIt is then extracted with ethyl acetate (3×50 ml)
  3. washThe combined organic extracts are washed with water (50 ml)
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated
  6. customcrystallized