反应详情

温度

20 °C

A mixture of 1-iodo-3-nitrobenzene (3 g), 6-bromohexyl but-3-ynyl ether (3 g), bis(triphenylphosphine)palladium (II) chloride (0.421 g), copper (I) iodide (0.114 g) in DMF (10 ml) and diisopropylethylamine (4 ml) was stirred under nitrogen at 20° C. for 5 h. The mixture was concentrated under reduced pressure and the residue was diluted in EtOAc and washed with 2M HCl, NaHCO3, brine and dried (MgSO4). The solvent was removed by evaporation and the residue was chromatographed on a Biotage column eluting with ether:petroleum ether(40–60° C.) (1:9) to give the title compound (4.12 g). LCMS RT=4.14 min

1. concentrationThe mixture was concentrated under reduced pressure
2. additionthe residue was diluted in EtOAc
3. washwashed with 2M HCl, NaHCO3, brine
4. dry with materialdried (MgSO4)
5. customThe solvent was removed by evaporation
6. customthe residue was chromatographed on a Biotage column
7. washeluting with ether