HRID1634886
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 100 °C
PROCEDURE
实验过程
Phosphorus oxychloride (2 mL) was added to 4-(3,4,5-Trimethoxyphenyl)pyridine-N-oxide (27 mg) at 0° C., and the mixture was stirred at 100° C. for 5 hours. The reaction mixture was concentrated under reduced pressure, and the residue was diluted with ethyl acetate and neutralized with a saturated aqueous solution of sodium hydrogencarbonate at 0° C. The neutralized product was extracted with ethyl acetate, and the extract was washed with saturated brine and dried over anhydrous sodium sulfate. The residue was purified by column chromatography on silica gel (ethyl acetate) to obtain the title compound.
WORKUP
后处理
- concentrationThe reaction mixture was concentrated under reduced pressure
- additionthe residue was diluted with ethyl acetate
- customneutralized with a saturated aqueous solution of sodium hydrogencarbonate at 0° C
- extractionThe neutralized product was extracted with ethyl acetate
- washthe extract was washed with saturated brine
- dry with materialdried over anhydrous sodium sulfate
- customThe residue was purified by column chromatography on silica gel (ethyl acetate)