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
To tert-butyl N-(3-{[(tert-butoxycarbonyl)sulfamoyl]amino}benzyl)-N-(trifluoroacetyl)glycinate (2.19 g) were added a 50% aqueous methanol solution (43.9 mL) and potassium carbonate (1.19 g), followed by stirring at room temperature for 5 hours. The reaction mixture was concentrated under reduced pressure, and then the residue was dissolved in water, followed by neutralization with 1 M hydrochloric acid. The mixture was extracted with a mixed solvent of n-butanol and ethyl acetate, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (methanol-chloroform) to obtain tert-butyl N-(3-{[(tert-butoxycarbonyl)sulfamoyl]amino}benzyl)glycinate (1.38 g).
WORKUP
后处理
- concentrationThe reaction mixture was concentrated under reduced pressure
- dissolutionthe residue was dissolved in water
- extractionThe mixture was extracted with a mixed solvent of n-butanol and ethyl acetate
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated under reduced pressure
- customThe residue was purified by silica gel column chromatography (methanol-chloroform)