HRID1533869

反应详情

EQUATION

反应方程式

HRID 1533869 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

3-(4-Methyl-1-piperazinyl)propoxyamine trihydrochloride may be obtained in the following manner: a solution of N-[3-(4-methyl-1-piperazinyl)propoxy]phthalimide (5.7 g) in 6 N hydrochloric acid (30 cc) is heated to reflux for 3 hours. After 18 hours' stirring at a temperature in the region of 20° C., the suspension obtained is filtered and the filtrate is concentrated to dryness under reduced pressure (20 mm Hg; 2.7 kPa) at a temperature in the region of 60° C. A crude product (6 g) is thereby obtained, which is resuspended in ethanol (30 cc). The crystals which appear are separated by filtration, washed 3 times with ethanol (45 cc in total) and then 3 times with ethyl ether (75 cc in total) and finally dried under reduced pressure (20 mm Hg; 2.7 kPa) at a temperature in the region of 20° C. 3-(4-Methyl-1-piperazinyl)propoxyamine trihydrochloride (3.4 g) is thereby obtained in the form of cream-coloured crystals, m.p. 240° C.

WORKUP

后处理

  1. temperatureto reflux for 3 hours
  2. customthe suspension obtained
  3. filtrationis filtered
  4. concentrationthe filtrate is concentrated to dryness under reduced pressure (20 mm Hg; 2.7 kPa) at a temperature in the region of 60° C
  5. customA crude product (6 g) is thereby obtained
  6. customThe crystals which appear are separated by filtration
  7. washwashed 3 times with ethanol (45 cc in total)
  8. dry with material3 times with ethyl ether (75 cc in total) and finally dried under reduced pressure (20 mm Hg; 2.7 kPa) at a temperature in the region of 20° C