HRID2303940

反应详情

EQUATION

反应方程式

HRID 2303940 的结构方程式

PROCEDURE

实验过程

m-Aminophenol (1.1 g, 10 mmol), 1-bromo-3-chloropropane (4.8 g, 3 ml, 30 mmol) and ethanol (10 ml) were placed in a 100 ml two-necked round-bottomed flask. The mixture was heated and refluxed for 11 hours, during which an NaHCO3 aqueous solution (2.0 g, 20 ml, 23 mmol) was added. The mixture was further heated and refluxed for 37 hours. The solvent was removed by distillation under reduced pressure. The resulting crude product was extracted with hexane by a solid-liquid continuous extraction to give 8-hydroxyjulolidine (661 mg) in 35% yield.

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. additionwas added
  3. temperatureThe mixture was further heated
  4. temperaturerefluxed for 37 hours
  5. customThe solvent was removed by distillation under reduced pressure
  6. extractionThe resulting crude product was extracted with hexane by a solid-liquid continuous extraction