HRID377022

反应详情

EQUATION

反应方程式

HRID 377022 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Sodium periodate (14.2 g) was dissolved in water (175 ml) and ruthenium trichloride (0.7 g) added to give a black solution. The solution was stirred during the addition of 3-(3-bromo-4-chlorophenyl)-5-hydroxythiazolidin-4-one (7.85 g) in methanol (35 ml) over 5 min, the reaction vessel was cooled in an ice bath to control the resulting exotherm. The mixture was stirred for 1 hour before quenching with sodium metabisulfite. The mixture was extracted with ethyl acetate and the combined organic extracts washed with aqueous sodium metabisulfite solution and water, then dried (MgSO4). Evaporation of the solvent under reduced pressure gave a gum which was triturated with dichloromethane to give the title compound as a grey solid (1.13 g), m.p. 139-140° C.

WORKUP

后处理

  1. customto give a black solution
  2. temperaturethe reaction vessel was cooled in an ice bath
  3. custombefore quenching with sodium metabisulfite
  4. extractionThe mixture was extracted with ethyl acetate
  5. washthe combined organic extracts washed with aqueous sodium metabisulfite solution and water
  6. dry with materialdried (MgSO4)
  7. customEvaporation of the solvent under reduced pressure
  8. customgave a gum which
  9. customwas triturated with dichloromethane