HRID1955004
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureAfter cooling to RT
- extractionIt is then extracted with ethyl acetate (3×50 ml)
- washThe combined organic extracts are washed with water (50 ml)
- dry with materialdried over magnesium sulfate
- concentrationconcentrated
- customcrystallized