HRID37512
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
- 60 °C
PROCEDURE
实验过程
A mixture of 0.30 g of 3,4-diethoxycarbonyl-2-mercapto-5-nitro-6-phenylpyridine, 0.41 g of reduced iron and 7 ml of ethanol was heated to 60° C., followed by addition of 1.7 ml of conc. hydrochloric acid. The mixture was heated under reflux for 30 minutes. After the reaction mixture was concentrated, the concentrate was extracted with ethyl acetate. The extract was washed with an aqueous solution of sodium chloride and dried over magnesium sulfate. The concentrate was subjected to silica gel column chromatography with chloroform as the eluent, to give 0.21 g of the title compound as a yellowish orange viscous oily substance.
WORKUP
后处理
- temperatureThe mixture was heated
- temperatureunder reflux for 30 minutes
- concentrationAfter the reaction mixture was concentrated
- extractionthe concentrate was extracted with ethyl acetate
- washThe extract was washed with an aqueous solution of sodium chloride
- dry with materialdried over magnesium sulfate