反应详情

温度

100 °C

To a solution of 4-chloro-2-(difluoromethyl)-1H-indole-5-carbonitrile (0.019 g, 0.084 mmol) in MeCN (2 mL), under N2, was added Cs2CO3 (0.055 g, 0.17 mmol) and 4-[(2-bromoethyl)oxy]phenyl methyl sulfone (0.047 g, 0.17 mmol). The mixture was heated in a sealed tube at 100° C. for 1 h. Upon cooling, the mixture was partitioned between EtOAc and water. The organic phase was washed with sat'd brine, dried (Na2SO4) and concentrated in vacuo. The residue was purified by flash chromatography (0-70% EtOAc-hexanes gradient) and the product was crystallized from CH2Cl2-hexanes to give the title compound as a white solid (0.022 g, 61% yield): MS (ES) m/z 425 (M+1).

1. temperatureUpon cooling
2. customthe mixture was partitioned between EtOAc and water
3. washThe organic phase was washed with sat'd brine
4. dry with materialdried (Na2SO4)
5. concentrationconcentrated in vacuo
6. customThe residue was purified by flash chromatography (0-70% EtOAc-hexanes gradient)
7. customthe product was crystallized from CH2Cl2-hexanes