HRID982844
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
- 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 1 N NaOH solution (20 ml) and extracted with ethyl acetate. The organic phase was 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
- temperatureunder reflux for 4 h
- filtrationthe precipitate was filtered off
- concentrationThe filtrate was concentrated
- customthe oily residue was quenched
- temperaturewith cooled 1 N NaOH solution (20 ml)
- extractionextracted with ethyl acetate
- washThe organic phase was washed with brine
- dry with materialdried over magnesium sulphate
- concentrationconcentrated to dryness