反应详情

温度

78 °C

A mixture of 4-[2-(tert-butoxycarbonylamino)ethyl]-phenyl trifluoromethanesulfonate (6.11 g, 16.6 mmol), palladium(II) acetate (745 mg, 3.32 mmol), 1,3-bis-(diphenylphosphino)propane (1.37 g, 3.32 mmol), triethylamine (6.94 ml, 49.8 mmol), and MeOH (24ml) in DMF (60 ml) was purged for 30 min with carbon monoxide. The mixture was stirred under carbon monoxide atmosphere at 78° C. for 3 hours. After cooling the mixture to room temperature, the reaction mixture was diluted with EtOAc, washed with water, 1N-hydrochloric acid, water, saturated sodium hydrogencarbonate, water and brine successively, dried over magnesium sulfate, and evaporated in vacuo. The residue was purified by silica gel column chromatography (hexane:EtOAc, 4:1-3:1) to give methyl 4-[2-(tert-butoxycarbonylamino)ethyl]benzoate (3.52 g, 76%).

1. customwas purged for 30 min with carbon monoxide
2. temperatureAfter cooling the mixture to room temperature
3. additionthe reaction mixture was diluted with EtOAc
4. washwashed with water, 1N-hydrochloric acid, water, saturated sodium hydrogencarbonate, water and brine successively
5. dry with materialdried over magnesium sulfate
6. customevaporated in vacuo
7. customThe residue was purified by silica gel column chromatography (hexane:EtOAc, 4:1-3:1)