HRID2111845

反应详情

EQUATION

反应方程式

HRID 2111845 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

Tropane (11.0 mL, 7.44 mmol) was dissolved in toluene (10 mL), chloroethyl carbonate (2.2 mL, 23 mmol) was added slowly, and the mixture stirred at 80° C. for 24 hours. Distilled water was added to the reaction mixture, and the mixture extracted with ethyl acetate. The organic phase was dried and concentrated by anhydrous magnesium sulfate. The obtained oily residue was dissolved in concentrated hydrochloric acid (10 mL), and heated with stirring at 100° C. for 2 hours. The solvent was distilled off under reduced pressure, toluene was added to the residue, and the mixture distilled under reduced pressure to obtain the target substance (820 mg, 72%) as a colorless solid.

WORKUP

后处理

  1. extractionthe mixture extracted with ethyl acetate
  2. customThe organic phase was dried
  3. concentrationconcentrated by anhydrous magnesium sulfate
  4. dissolutionThe obtained oily residue was dissolved in concentrated hydrochloric acid (10 mL)
  5. temperatureheated
  6. stirringwith stirring at 100° C. for 2 hours
  7. distillationThe solvent was distilled off under reduced pressure, toluene
  8. additionwas added to the residue
  9. distillationthe mixture distilled under reduced pressure
  10. customto obtain the target substance (820 mg, 72%) as a colorless solid