HRID2223824

反应详情

EQUATION

反应方程式

HRID 2223824 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureThe reaction solution was cooled down to room temperature
  2. extractionextracted with chloroform
  3. washThe organic layer was washed with 5% citric acid and saturated brine
  4. customdried
  5. customThe solvent was evaporated under a reduced pressure
  6. washeluted with ethyl acetate:n-hexane (2:1)
  7. customthe thus obtained crude product
  8. customwas crystallized from ethyl acetate/n-hexane