HRID533682

反应详情

EQUATION

反应方程式

HRID 533682 的结构方程式

PROCEDURE

实验过程

The steps are: add 3-(3-methoxy-phenyl)-N,N,2-trimethyl pentylamine into a reaction flask, add hydroiodic acid, and perform heating and reflux for 5 hours; detect the reaction process by TLC; after that, cool the resultant to the room temperature, pour it to an alkaline solution to make the pH become 9, perform extraction by ethyl acetate and rinse by water; recycle the solvent by drying and decompression to obtain a light yellow liquid, 3-(3-hydroxy-phenyl)-N,N,2-trimethyl pentylamine; and separate the mother solution by a separator, form the salt by the acidification of hydrochloric acid to obtain tapentadol hydrochloride. HPLC: 99.56%, ee %>99.5%.

WORKUP

后处理

  1. temperatureperform heating
  2. temperaturereflux for 5 hours
  3. additionpour it to an alkaline solution
  4. extractionextraction by ethyl acetate
  5. washrinse by water
  6. customby drying