HRID1478678
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
- 20 °C
PROCEDURE
实验过程
A solution of ethyl 5-methylimidazo[1,2-a]pyridine-2-carboxylate (5.0 g, 25 mmol) in acetonitrile (94 mL) was treated with N-bromosuccinimide (4.8 g, 27 mmol) in acetonitrile (47 mL) dropwise and stirred at 20° C. for 30 min. The reaction mixture was concentrated, diluted with dichloromethane (200 mL), and washed with saturated sodium bicarbonate (150 mL) and brine (50 mL). The organic layer was dried with sodium sulfate, filtered, and concentrated to a crude solid. Purification by flash column chromatography gave the desired product (4.0 g, 58%). LCMS for C11H12BrN2O2 (M+H)+: m/z=282.9, 284.9.
WORKUP
后处理
- concentrationThe reaction mixture was concentrated
- additiondiluted with dichloromethane (200 mL)
- washwashed with saturated sodium bicarbonate (150 mL) and brine (50 mL)
- dry with materialThe organic layer was dried with sodium sulfate
- filtrationfiltered
- concentrationconcentrated to a crude solid
- customPurification by flash column chromatography