HRID70541
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
- 110 °C
PROCEDURE
实验过程
Palladium acetate (36 mg) was added to a suspension of 6-bromo-3-iodo-2-methoxypyridine (1.0 g), cyclopropylboronic acid (547 mg), triphenylphosphine (84 mg) and potassium carbonate (1.32 g) in toluene (20 mL) and water (1 mL), and the mixture was stirred at 110° C. for 4.5 hours. Water and ethyl acetate were added to the reaction solution, followed by extraction with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate and filtered. The filtrate was concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=99:1→96:4) to give the title compound as a colorless oil (782 mg).
WORKUP
后处理
- extractionfollowed by extraction with ethyl acetate
- dry with materialThe organic layer was dried over anhydrous magnesium sulfate
- filtrationfiltered
- concentrationThe filtrate was concentrated under reduced pressure
- customThe resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=99:1→96:4)