HRID1078409

反应详情

EQUATION

反应方程式

HRID 1078409 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureOn cooling
  2. additionwas added
  3. temperatureunder reflux for 6 hours
  4. filtrationthe mixture was filtered
  5. customthe filtrate evaporated to dryness under reduced pressure
  6. additionThe residue was treated with water (16 ml)
  7. temperaturethen cooled
  8. additionsodium hydroxide (24 g) added in portions
  9. extractionThe solution was extracted with diethyl ether
  10. customThe combined organic extracts were dried
  11. customevaporated
  12. customto give an oil which
  13. distillationwas distilled under reduced pressure