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
- 95 °C
PROCEDURE
实验过程
A mixture of N-[3-(2-phenylimidazol-1-yl)propyl]phthalimide (17.0 g), sodium hydroxide (1.1 g) and water (5.4 ml) was heated at 95° C. for 48 hours. On cooling, a mixture of concentrated hydrochloric acid (66 ml) and water (13 ml) was added and the mixture boiled under reflux for 6 hours. After standing at ambient temperature for 16 hours, the mixture was filtered and the filtrate evaporated to dryness under reduced pressure. The residue was treated with water (16 ml) then cooled and sodium hydroxide (24 g) added in portions. The solution was extracted with diethyl ether and then with dichloromethane. The combined organic extracts were dried and evaporated to give an oil which was distilled under reduced pressure to give 3-(2-phenylimidazol-1-yl)propylamine, b.p. 128° C. (0.05 mmHg).
WORKUP
后处理
- temperatureOn cooling
- additionwas added
- temperatureunder reflux for 6 hours
- filtrationthe mixture was filtered
- customthe filtrate evaporated to dryness under reduced pressure
- additionThe residue was treated with water (16 ml)
- temperaturethen cooled
- additionsodium hydroxide (24 g) added in portions
- extractionThe solution was extracted with diethyl ether
- customThe combined organic extracts were dried
- customevaporated
- customto give an oil which
- distillationwas distilled under reduced pressure