HRID1452560

反应详情

EQUATION

反应方程式

HRID 1452560 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

(5S)-5-(Azidomethyl)-3-[4-(1,1-dioxo-3,6-dihydro-2H-thiopyran-4-yl)-3,5-difluorophenyl]-1,3-oxazolidin-2-one (WO 01/81350 A1) (7 g, 18.2 mmol) was dissolved in water (15 ml) and acetonitrile (150 ml). Triphenylphosphine (5.73 g, 21.9 mmol) was added and the resulting mixture was stirred at room temperature for 2 hours. The solvent was evaporated and the residue purified by flash column chromatography on silica gel with 5% methanol in dichloromethane. The fractions containing product were evaporated to near dryness and treated with ethereal HCl to precipitate the hydrochloride salt of the title compound as a white solid (5.03 g, 70%).

WORKUP

后处理

  1. customThe solvent was evaporated
  2. customthe residue purified by flash column chromatography on silica gel with 5% methanol in dichloromethane
  3. additionThe fractions containing product
  4. customwere evaporated
  5. additiontreated with ethereal HCl
  6. customto precipitate the hydrochloride salt of the title compound as a white solid (5.03 g, 70%)