HRID1097383
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
5,6,6a,7,8,9-Hexahydro-4H-2-phenalenylamine (0.100 g) was added with ethyl 2-chloropyrimidine-5-carboxylate (0.101 g) and potassium carbonate (0.400 g), and the mixture was stirred overnight at 110° C. The reaction mixture was left to cool and then added with water, and the mixture was extracted with chloroform. The organic layer was washed successively with water and saturated brine, and dried over anhydrous sodium sulfate. The organic layer was concentrated under reduced pressure, and the resulting residue was purified by silica gel column chromatography (developing solvent: ethyl acetate:n-hexane=1:20) to obtain the title compound (0.167 g, yield: 93%).
WORKUP
后处理
- waitThe reaction mixture was left
- temperatureto cool
- extractionthe mixture was extracted with chloroform
- washThe organic layer was washed successively with water and saturated brine
- dry with materialdried over anhydrous sodium sulfate
- concentrationThe organic layer was concentrated under reduced pressure
- customthe resulting residue was purified by silica gel column chromatography (developing solvent: ethyl acetate:n-hexane=1:20)