HRID1047588

反应详情

EQUATION

反应方程式

HRID 1047588 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. stirringstirred at 25°˜30° C. for 8-10 hours
  2. customExcess hydrochloric acid gas was removed by concentration of the solvent
  3. customto give a solid
  4. temperatureThe reaction mass was cooled to 0-5° C
  5. stirringwas stirred for 1 h at 25° C
  6. customThe solid obtained
  7. filtrationwas filtered
  8. washwas washed with ethyl acetate (1000 ml)
  9. customThe solid obtained
  10. customwas dried for 6 h under vacuum at 55° C.-60° C.