HRID2111845
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
- 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
- extractionthe mixture extracted with ethyl acetate
- customThe organic phase was dried
- concentrationconcentrated by anhydrous magnesium sulfate
- dissolutionThe obtained oily residue was dissolved in concentrated hydrochloric acid (10 mL)
- temperatureheated
- stirringwith stirring at 100° C. for 2 hours
- distillationThe solvent was distilled off under reduced pressure, toluene
- additionwas added to the residue
- distillationthe mixture distilled under reduced pressure
- customto obtain the target substance (820 mg, 72%) as a colorless solid