HRID414123

反应详情

EQUATION

反应方程式

HRID 414123 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A 2 g quantity of benzyl 2-(3-phenoxyacetamido-4-benzenesulfonylthio-2-azetidinone-1-yl)-3-methyl-3-butenate was dissolved in 12 ml of ethoxyethyl acetate. To the solution was added 6 g of NaHCO3 and the mixture was stirred at room temperature. Thereto was added dropwise over 1 hour 12.1 ml of a 0.285M solution of Cl2O in carbon tetrachloride. Water was added to the reaction mixture and the mixture was extracted with ethyl acetate and dried over anhydrous magnesium sulfate. The solvent was distilled off at reduced pressure. The resulting residue was separated and purified by silica gel column chromatography, giving 2.0 g of benzyl 2-(3-phenoxyacetamido-4-benzenesulfonylthio-2-azetidinone-1-yl)-3-chloromethyl-3-butenate in 94% yield.

WORKUP

后处理

  1. extractionthe mixture was extracted with ethyl acetate
  2. dry with materialdried over anhydrous magnesium sulfate
  3. distillationThe solvent was distilled off at reduced pressure
  4. customThe resulting residue was separated
  5. custompurified by silica gel column chromatography