反应详情

305.7 mg N-(4-hydroxynaphthalen-1-yl)thiophene-2-sulfonamide (3) was dissolved in 1 ml DMF, to which at 0° C. was added 320 mg Br2 in 1 ml dichloromethylene solution. After stirred at r.t. for 1 h, 558 μl TEA was added at 0° C. The reaction was stirred at r.t. overnight and diluted with ethyl acetate to 50 ml. The organic phase was washed with water and brine. Dried over Na2SO4, the organic phase was filtered and concentrated. The crude product was purified via flash chromatography (Hex/EtOAc gradient) affording an orange-red solid 140 mg (36.4%), m.p.: 128-130° C.

1. stirringThe reaction was stirred at r.t. overnight
2. washThe organic phase was washed with water and brine
3. dry with materialDried over Na2SO4
4. filtrationthe organic phase was filtered
5. concentrationconcentrated
6. customThe crude product was purified via flash chromatography (Hex/EtOAc gradient)