反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of {3-{[2-(4,5-diphenyloxazol-2-yl)-2-cyclohexen-1-yl]methyl}phenyl}carbamic acid tert-butyl ester (2.34 g, 4.62 mmol) in methylene chloride (25 ml) was added trifluoroacetic acid (7 ml) at 5° C. and the mixture was stirred at room temperature for 1.5 hour. After evaporation, the residue was dissolved in EtOAc, and saturated sodium hydrogencarbonate solution was added thereto under ice-cooling. The mixture was extracted with EtOAc, washed with water and brine, dried over magnesium sulfate, and evaporated in vacuo. The residue was purified by silica gel column chromatography (hexane:EtOAc, 3:1 elution) to give 3-{[2-(4,5-diphenyloxazol-2-yl)-2-cyclohexen-1-y]methyl}phenylamine (1.74 g, 93%).
WORKUP
后处理
- customAfter evaporation
- dissolutionthe residue was dissolved in EtOAc
- additionsaturated sodium hydrogencarbonate solution was added
- temperatureunder ice-cooling
- extractionThe mixture was extracted with EtOAc
- washwashed with water and brine
- dry with materialdried over magnesium sulfate
- customevaporated in vacuo
- customThe residue was purified by silica gel column chromatography (hexane:EtOAc, 3:1 elution)