HRID1423032
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
PROCEDURE
实验过程
A mixture of imidazo[1,2-a]pyridine-8-carboxylic acid methyl ester (3.24 g, 18.3 mmol) and N-iodosuccinimide (NIS) (4.11 g, 18.3 mmol) in acetonitrile (50 mL) is stirred at room temperature. After 2 hours, the reaction mixture is quenched with saturated aqueous Na2S2O3 and extracted with EtOAc (3×100 mL). The combined organic layers are washed with water, brine, dried over Na2SO4 and concentrated. The crude material is purified by silica gel chromatography eluting with 80% EtOAc in hexanes to afford 3-iodo-imidazo[1,2-a]pyridine-8-carboxylic acid methyl ester. Mp: 99-110° C.
WORKUP
后处理
- customthe reaction mixture is quenched with saturated aqueous Na2S2O3
- extractionextracted with EtOAc (3×100 mL)
- washThe combined organic layers are washed with water, brine
- dry with materialdried over Na2SO4
- concentrationconcentrated
- customThe crude material is purified by silica gel chromatography
- washeluting with 80% EtOAc in hexanes