反应详情

温度

70 °C

To a mixture of sodium azide (0.061 g, 0.95 mmol) and aluminum trichloride (0.042 g, 0.31 mmol) was added 3-(5-chloro-2-{2-[4-(4-fluoro-benzyl)-(2R,5S)-2,5-dimethyl-piperazin-1-yl]-2-oxo-ethoxy}-phenyl)-3-oxo-propionitrile (0.035 g, 0.076 mmol) in tetrahydrofuran (2 mL). The reaction was warmed to 70° C. and stirred for 18 hours. To this was added saturated aqueous sodium bicarbonate (0.5 mL) and dimethylsulfoxide (0.5 mL) and the solution was stirred for 1 hour at ambient temperature. The solids were removed by filtration and the filtrate was concentrated in vacuo. The crude product was purified by reverse phase HPLC to give the title compound which was converted to its hydrochloride salt (0.020 g, LRMS: 501.2).

1. stirringthe solution was stirred for 1 hour at ambient temperature
2. customThe solids were removed by filtration
3. concentrationthe filtrate was concentrated in vacuo
4. customThe crude product was purified by reverse phase HPLC