反应详情

To a solution of methyl 3,5-bis[(1E)-3-methoxyprop-1-en-1-yl]benzoate (1 eq.) from the previous step in refluxing toluene was added benzenesulfonohydrazide (5 eq) in five portions over 2 h. The reaction was stirring as reflux for 18 h. After cooling to rt, the reaction was diluted with ether. The organic extract was washed with 1 N aqueous HCl, brine, dried over MgSO4, and concentrated in vacuo. The crude product was purified by flash column chromatography (SiO2, 20% EtOAc in Hex) to afford the title compound as an oil.

1. temperatureas reflux for 18 h
2. extractionThe organic extract
3. washwas washed with 1 N aqueous HCl, brine
4. dry with materialdried over MgSO4
5. concentrationconcentrated in vacuo
6. customThe crude product was purified by flash column chromatography (SiO2, 20% EtOAc in Hex)