HRID1579856

反应详情

EQUATION

反应方程式

HRID 1579856 的结构方程式

PROCEDURE

实验过程

A solution of 60.9 g (0.31 mole) of phenacyl bromide in 150 ml. of toluene was added dropwise with stirring to a refluxing solution of 46.6 g. of 1-pyrrolidino-1-cyclohexene in 150 ml. of toluene. The mixture was heated under reflux for 2 hours, diluted with 150 ml. of water, refluxed for 3 hours and cooled. The layers were separated, and the aqueous phase was extracted with ether. The organic solution was dried and concentrated to an oil. Distillation gave 42.1 g. (64%) of orange liquid, b.p. 135°-141° (0.05 mm.), which solidified. Recrystallization from ether-petroleum ether gave tan crystals, m.p. 44°-45°.

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 2 hours
  3. additiondiluted with 150 ml
  4. temperaturecooled
  5. customThe layers were separated
  6. extractionthe aqueous phase was extracted with ether
  7. customThe organic solution was dried
  8. concentrationconcentrated to an oil
  9. distillationDistillation
  10. customgave 42.1 g
  11. customRecrystallization from ether-petroleum ether
  12. customgave tan crystals, m.p. 44°-45°