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
7-bromoimidazo[1,2-a]pyridine-3-carboxylic acid (4.93 g, 20.5 mmol) was dissolved in 80 mL of dry dichloromethane. To this solution was added oxalyl chloride (20.5 mL, 40.9 mmol, 2M in dichloromethane) followed by a few drops of DMF. The mixture was stirred at ambient temperature for 16 hours, then concentrated under reduced pressure. The resulting material was taken up in 100 mL of methanol and stirred at ambient temperature for 6 hours, then concentrated under reduced pressure. The resulting material was suspended in saturated aqueous sodium bicarbonate, extracted with dichloromethane and EtOAc. The organics were combined, dried over sodium sulfate and concentrated under reduced pressure to give 4.63 g (89%) of the title compound.
WORKUP
后处理
- concentrationconcentrated under reduced pressure
- stirringstirred at ambient temperature for 6 hours
- concentrationconcentrated under reduced pressure
- extractionextracted with dichloromethane and EtOAc
- dry with materialdried over sodium sulfate
- concentrationconcentrated under reduced pressure