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
Palladium acetate (267 mg), 1,1′-bis(diphenylphosphino)ferrocene (1.3 g) and triethylamine (3.2 mL) were added to an ethanol-DMF mixed solvent (1/1, 20 mL) of 6-chloropyridin-3-ol (1.5 g), and stirred overnight in a carbon monoxide atmosphere (1 atmospheric pressure) at 50° C. Ethanol was evaporated off under reduced pressure from the reaction solution, water was added to the resulting residue, and extracted with chloroform/methanol (10/1). The organic layer was dried with anhydrous magnesium sulfate, and the solvent was evaporated off under reduced pressure. The resulting residue was purified through silica gel column chromatography (hexane/ethyl acetate=2/3) to obtain the entitled compound (500 mg).
WORKUP
后处理
- customEthanol was evaporated off under reduced pressure from the reaction solution, water
- additionwas added to the resulting residue
- extractionextracted with chloroform/methanol (10/1)
- dry with materialThe organic layer was dried with anhydrous magnesium sulfate
- customthe solvent was evaporated off under reduced pressure
- customThe resulting residue was purified through silica gel column chromatography (hexane/ethyl acetate=2/3)