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
PROCEDURE
实验过程
To a solution of N-[3-(4-isopropyl-1-piperazinyl)propyl]phthalimide (43.1 g) in ethanol (350 ml) was added 100% hydrazine hydrate (11.2 g). The resulting mixture was refluxed with stirring for 3 hours. The reaction mixture was cooled and then filtered. The filter cake was washed with ethanol. The filtrate and washing were combined and concentrated under reduced pressure. The residual oil was subjected to column chromatography (aluminum oxide), eluting with a mixture of chloroform and methanol (20:1). The fractions containing the object compound were collected and then evaporated under reduced pressure. The residual oil was distilled under reduced pressure to give 3-(4-isopropyl-1-piperazinyl)propylamine (15.0 g), (bp 45 mmHg/150° C.).
WORKUP
后处理
- temperatureThe resulting mixture was refluxed
- temperatureThe reaction mixture was cooled
- filtrationfiltered
- washThe filter cake was washed with ethanol
- washThe filtrate and washing
- concentrationconcentrated under reduced pressure
- washeluting with a mixture of chloroform and methanol (20:1)
- additionThe fractions containing the object compound
- customwere collected
- customevaporated under reduced pressure
- distillationThe residual oil was distilled under reduced pressure