反应详情

温度

80 °C

A mixture of 3-{(2-(4,5-diphenyloxazol-2-yl)-2-cyclohexen-1-yl]methyl}benzoic acid (2.60 g, 5.98 mmol), triethylamine (1.08 ml, 7.77 mmol), and diphenylphosphoryl azide (1.67 ml, 7.77 mmol) in t-butanol-toluene (2:1, 80 ml) was stirred at 80° C. for 18 hours. After cooling the mixture to room temperature, the mixture was evaporated, diluted with EtOAc, washed with saturated sodium hydrogencarbonate solution, water and brine, dried over magnesium sulfate, and evaporated in vacuo. The residue was purified by silica gel column chromatography (hexane:EtOAc, 8:1 elution) to give {3-{[2-(4,5-diphenyloxazol-2-yl)-2-cyclohexen-1-yl]methyl}phenyl}carbamic acid tert-butyl ester (2.36 g, 78%).

1. temperatureAfter cooling the mixture to room temperature
2. customthe mixture was evaporated
3. additiondiluted with EtOAc
4. washwashed with saturated sodium hydrogencarbonate solution, water and brine
5. dry with materialdried over magnesium sulfate
6. customevaporated in vacuo
7. customThe residue was purified by silica gel column chromatography (hexane:EtOAc, 8:1 elution)