HRID2206247
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 65 °C
PROCEDURE
实验过程
To a mixture of methyl 1-(4-nitrophenyl)piperidine-4-carboxylate (3.80 g) and iron powder (3.20 g) in methanol/water (40 mL/10 mL) was added conc. hydrochloric acid (2 mL) at room temperature. The reaction mixture was stirred at 65° C. for 3 hr. The reaction mixture was adjusted to pH=9 with saturated sodium carbonate, and the insoluble substance was removed by the filtration. The filtrate was concentrated under reduced pressure, and the residue was extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure to give the title compound (3.20 g).
WORKUP
后处理
- customthe insoluble substance was removed by the filtration
- concentrationThe filtrate was concentrated under reduced pressure
- extractionthe residue was extracted with ethyl acetate
- washThe organic layer was washed with saturated brine
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated under reduced pressure