HRID875299

反应详情

EQUATION

反应方程式

HRID 875299 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
22.5 °C

PROCEDURE

实验过程

Tapentadol free base (2.1 g) was added to 2-butanone (32 ml), the mixture was heated to reflux and followed by the addition of water (0.22 ml) and trimethylchlorosilane (1.6 ml) at the same temperature and then maintaining for 1 hour. The resulting mass was cooled at 20-25° C. The resulting solid was filtered, the product was washed with pre-cooled 2-butanone (4 ml) and then the solid was dried at 25° C. for 3 hours to produce 1.8 g of tapentadol hydrochloride salt (Purity by HPLC: 97.78%).

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureto reflux
  3. temperaturemaintaining for 1 hour
  4. filtrationThe resulting solid was filtered
  5. washthe product was washed with pre-cooled 2-butanone (4 ml)
  6. customthe solid was dried at 25° C. for 3 hours