HRID1042122
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
To a solution of 4-(5-fluoro-2-nitrophenoxy)tetrahydro-2H-pyran (19.5 g) and 6-(methylsulfonyl)pyridin-3-ol (14 g) in N,N-dimethylformamide (250 mL) was added potassium carbonate (22.3 g), and the mixture was stirred at 110° C. for 4 hr. 1N HCl was added to the reaction solution, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over magnesium sulfate, filtered and concentrated under reduced pressure. The obtained crude product was subjected to silica gel column chromatography (ethyl acetate:hexane=0:100 to 50:50, volume ratio) to give the title compound (26.4 g, yield 83%) as a yellow solid.
WORKUP
后处理
- extractionthe mixture was extracted with ethyl acetate
- washThe organic layer was washed with saturated brine
- dry with materialdried over magnesium sulfate
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customThe obtained crude product