HRID1654222

反应详情

EQUATION

反应方程式

HRID 1654222 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In dichloromethane (1.5 ml) was dissolved (2R,3R)-2-(2,4-difluorophenyl)-3-mercapto-1-(1H-1,2,4-triazol-1-yl)-2-butanol (60 mg), followed by addition of triethylamine (33 ml) and acetyl chloride (13 ml) under ice-cooling. The mixture was then stirred at room temperature for 30 minutes, and then the solvent was distilled off under reduced pressure. The residue was purified by silica gel chromatography (eluent: hexane-ethyl acetate=1:2) and the desired fraction was concentrated to give (2R,3R)-3-acetylthio-2-(2,4-difluorophenyl)-1-(1H-1,2,4-triazol-1-yl)-2-butanol (compound 45:59 mg) as a colorless solid.

WORKUP

后处理

  1. temperaturecooling
  2. distillationthe solvent was distilled off under reduced pressure
  3. customThe residue was purified by silica gel chromatography (eluent: hexane-ethyl acetate=1:2)
  4. concentrationthe desired fraction was concentrated