反应详情

温度

125 °C

A mixture of 4-[4-(t-butoxycarbonyl)piperazin-1-yl]-3-iodo-1H-indazole (0.110 g, 0.257 mmol), sodium benzene sulfinate (0.068 g, 0.411 mmol), copper(I) iodide (0.073 g, 0.386 mmol) and N,N-dimethylformamide is added to a screw-capped test-tube with Teflon-lined septum. The tube is evacuated and backfilled with argon. This procedure is repeated twice, then the tube is heated to 125° C. for 4 h. The reaction mixture is cooled, partitioned between ethyl acetate and water and filtered through a pad of diatomaceous earth. The filtrate is separated. The organic phase is washed with brine, dried over sodium sulfate and concentrated in vacuo. The resulting crude material is purified by column chromatography (silica gel, 40:60 ethyl acetate/hexanes) to afford the title compound as a pale yellow foam, 0.022 g (18% yield), identified by NMR and mass spectral analyses.

1. customThe tube is evacuated
2. temperatureThe reaction mixture is cooled
3. custompartitioned between ethyl acetate and water
4. filtrationfiltered through a pad of diatomaceous earth
5. customThe filtrate is separated
6. washThe organic phase is washed with brine
7. dry with materialdried over sodium sulfate
8. concentrationconcentrated in vacuo
9. customThe resulting crude material is purified by column chromatography (silica gel, 40:60 ethyl acetate/hexanes)