HRID2252829

反应详情

EQUATION

反应方程式

HRID 2252829 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

Under an N2 atmosphere, 250 mg (0.93 mmol) of 1-chloro-4-(2-pyridin-3-yl-ethyl)isoquinoline in 2.9 ml of abs. ethanol are mixed with 131 mg (1.02 mmol) of 4-chloro-aniline and 0.23 ml of 4 N HCl/dioxane, and stirred for 8 h at 80° C. The mixture is cooled to RT, filtered and the residue washed with acetonitrile. The residue is dissolved in 4 ml of water, then 0.9 ml of sat. NH3 solution are added, stirring is effected for 10 min, the precipitate is filtered off and washed with water. Recrystallisation from acetonitrile yields 1-(4chloroanilino)-4-[2-(pyridin-3-yl)-ethyl]-isoquinoline; m.p.157-158° C.

WORKUP

后处理

  1. temperatureThe mixture is cooled to RT
  2. filtrationfiltered
  3. washthe residue washed with acetonitrile
  4. dissolutionThe residue is dissolved in 4 ml of water
  5. addition0.9 ml of sat. NH3 solution are added
  6. stirringstirring
  7. waitis effected for 10 min
  8. filtrationthe precipitate is filtered off
  9. washwashed with water
  10. customRecrystallisation from acetonitrile