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
6-Fluoro-2-iodo-3-methoxypyridine (52 mg), tetrakistriphenylphosphine palladium(0) (24 mg), and 3-pyridineboronic acid (76 mg) were suspended in a mixed solvent composed of N,N-dimethylformamide (0.75 ml) and a 2 N aqueous potassium carbonate solution (0.75 ml), and the suspension was stirred at 80° C. for 4 hr. The reaction solution was cooled to room temperature, the reaction solution was then filtered, and the solvent was removed from the filtrate by distillation under the reduced pressure. Water was then added to the residue, and the mixture was extracted with dichloromethane. The dichloromethane layer was washed with water and saturated brine and was dried over anhydrous magnesium sulfate. The solvent was removed by distillation under the reduced pressure, and the residue was purified by thin layer chromatography using acetone-chloroform to give 6-fluoro-3-methoxy-[2,3′]bipyridine (31 mg, yield 72%).
WORKUP
后处理
- filtrationthe reaction solution was then filtered
- customthe solvent was removed from the filtrate by distillation under the reduced pressure
- additionWater was then added to the residue
- extractionthe mixture was extracted with dichloromethane
- washThe dichloromethane layer was washed with water and saturated brine
- dry with materialwas dried over anhydrous magnesium sulfate
- customThe solvent was removed by distillation under the reduced pressure
- customthe residue was purified by thin layer chromatography