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
- 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
- temperatureto reflux for 3 hours
- customthe suspension obtained
- filtrationis filtered
- concentrationthe filtrate is concentrated to dryness under reduced pressure (20 mm Hg; 2.7 kPa) at a temperature in the region of 60° C
- customA crude product (6 g) is thereby obtained
- customThe crystals which appear are separated by filtration
- washwashed 3 times with ethanol (45 cc in total)
- 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