HRID1716552

反应详情

EQUATION

反应方程式

HRID 1716552 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
2.5 °C

PROCEDURE

实验过程

To a solution of 2-[3-(2-phenyl-1H-imidazol-4-yl)-propyl]-isoindole-1,3-dione (4.16 g) in ethanol (50 ml) was added hydrazine hydrate (3.18 g). The reaction mixture was stirred under reflux for 4 h, cooled down to 0-5° C., and the precipitate was filtered off. The filtrate was concentrated, and the oily residue was quenched with cooled 1N NaOH solution (20 ml) and extracted with ethyl acetate. The organic phase washed with brine, dried over magnesium sulphate and concentrated to dryness to obtain 3-(2-phenyl-1H-imidazol-4-yl)-propylamine (1.95 g) as a yellow foam, which was sufficiently pure to be used directly in the next step.

WORKUP

后处理

  1. temperatureunder reflux for 4 h
  2. filtrationthe precipitate was filtered off
  3. concentrationThe filtrate was concentrated
  4. customthe oily residue was quenched
  5. temperaturewith cooled 1N NaOH solution (20 ml)
  6. extractionextracted with ethyl acetate
  7. washThe organic phase washed with brine
  8. dry with materialdried over magnesium sulphate
  9. concentrationconcentrated to dryness