HRID1457262

反应详情

EQUATION

反应方程式

HRID 1457262 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of (2R,3S)-3-(4-methoxyphenyl)-2,3-epoxypropionamide and xylene is refluxed with heating under nitrogen atmosphere. When the reflux is started, a solution of 2-(2-dimethylaminoethylamino)thiophenol and ferrous sulfate heptahydrate in methanol is added immediately into the reaction mixture, and the mixture is reacted at the same temperature, and cooled to room temperature. The reaction mixture is concentrated under reduced pressure, and the residue is dissolved with heating in ethanol and water. The mixture is allowed to cool to 0° C., and the precipitated crystals are collected by filtration, washed with chilled 50% ethanol, and dried to give (2S,3S)-3-[2-(2-dimethylaminoethylamino)phenylthio]-2-hydroxy-3-(4-methoxyphenyl)propionamide.

WORKUP

后处理

  1. temperatureis refluxed
  2. temperaturewith heating under nitrogen atmosphere
  3. customthe mixture is reacted at the same temperature
  4. concentrationThe reaction mixture is concentrated under reduced pressure
  5. dissolutionthe residue is dissolved
  6. temperaturewith heating in ethanol
  7. temperatureto cool to 0° C.
  8. filtrationthe precipitated crystals are collected by filtration
  9. washwashed
  10. temperaturewith chilled 50% ethanol
  11. customdried