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
5-Methyl-5-phenyl-3-phenylamino-2-thioxothiazolidin-4-one (0.3 g) was added to a 1M methylene chloride solution of triethyloxonium tetrafluoroborate (1 ml) at room temperature with stirring. After stirring the mixture for 24 hrs hydroxylamine hydrochloride (0.1 g) and triethylamine (0.3 g) in methanol (10 ml) were added at 0° C. The reaction mixture was again stirred for 2 hrs at room temperature followed by evaporation of the solvents under reduced pressure. The residue was added to ice water and then extracted with ethyl acetate. The ethyl acetate solution was dried over anhydrous ethyl acetate and the solvent was then evaporated under reduced pressure. The residue was purified by column chromatography (ethyl acetate-n-hexane, ½) to yield 2-hydroxyimino-5-methyl-5-phenyl-3-phenylaminothiazolidine-4-one (0.21 g) having a melting point of 62-63° C.
WORKUP
后处理
- additionwere added at 0° C
- stirringThe reaction mixture was again stirred for 2 hrs at room temperature
- customfollowed by evaporation of the solvents under reduced pressure
- additionThe residue was added to ice water
- extractionextracted with ethyl acetate
- dry with materialThe ethyl acetate solution was dried over anhydrous ethyl acetate
- customthe solvent was then evaporated under reduced pressure
- customThe residue was purified by column chromatography (ethyl acetate-n-hexane, ½)