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
- 80 °C
PROCEDURE
实验过程
A 200 mg portion of 6-chloro-N,N′-diphenyl-1,3,5-triazine-2,4-diamine was dissolved in 10.0 ml of acetonitrile, and 145 mg of 4-(aminomethyl)pyridine and 0.585 ml of diisopropylethylamine were added thereto and stirred overnight at 80° C. The reaction solution was cooled down to room temperature, and then mixed with water and extracted with chloroform. The organic layer was washed with 5% citric acid and saturated brine and then dried using anhydrous magnesium sulfate. The solvent was evaporated under a reduced pressure, the thus obtained residue was applied to a silica gel column chromatography and eluted with ethyl acetate:n-hexane (2:1), and then the thus obtained crude product was crystallized from ethyl acetate/n-hexane, thereby obtaining 107 mg of N,N′-diphenyl-N″-(4-pyridylmethyl)-1,3,5-triazine-2,4,6-triamine as light red crystals.
WORKUP
后处理
- temperatureThe reaction solution was cooled down to room temperature
- extractionextracted with chloroform
- washThe organic layer was washed with 5% citric acid and saturated brine
- customdried
- customThe solvent was evaporated under a reduced pressure
- washeluted with ethyl acetate:n-hexane (2:1)
- customthe thus obtained crude product
- customwas crystallized from ethyl acetate/n-hexane