反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customto give a black solution
- temperaturethe reaction vessel was cooled in an ice bath
- custombefore quenching with sodium metabisulfite
- extractionThe mixture was extracted with ethyl acetate
- washthe combined organic extracts washed with aqueous sodium metabisulfite solution and water
- dry with materialdried (MgSO4)
- customEvaporation of the solvent under reduced pressure
- customgave a gum which
- customwas triturated with dichloromethane