HRID1047588
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
- 12.5 °C
PROCEDURE
实验过程
Ethyl acetate (810 ml) containing 10% HCl was added to the crude benzphetamine free base isolated from Example 1 at 10-15° C. The mixture was stirred for 30 min at 10-15° C. and then stirred at 25°˜30° C. for 8-10 hours. Excess hydrochloric acid gas was removed by concentration of the solvent to give a solid. The reaction mass was cooled to 0-5° C. Ethyl acetate (1500 ml) was added to the mixture and was stirred for 1 h at 25° C. The solid obtained was filtered and was washed with ethyl acetate (1000 ml). The solid obtained was dried for 6 h under vacuum at 55° C.-60° C.
WORKUP
后处理
- stirringstirred at 25°˜30° C. for 8-10 hours
- customExcess hydrochloric acid gas was removed by concentration of the solvent
- customto give a solid
- temperatureThe reaction mass was cooled to 0-5° C
- stirringwas stirred for 1 h at 25° C
- customThe solid obtained
- filtrationwas filtered
- washwas washed with ethyl acetate (1000 ml)
- customThe solid obtained
- customwas dried for 6 h under vacuum at 55° C.-60° C.