反应详情

温度

70 °C

(Step 2) To a suspension of 2-cyano-2-(3,4-dichloro-5-oxo-2,5-dihydrofuran-2-yl)acetamide (0.73 g) and 3-(aminomethyl)-N,N-dimethylbenzenesulfonamide obtained in Step 1 (1.0 g) in ethanol (10 ml) was added potassium carbonate (0.65 g) at room temperature, and the mixture was stirred overnight at 70° C. The reaction solution was filtered through celite. The solvent was evaporated under reduced pressure. The residue was purified by basic silica gel column chromatography (ethyl acetate:hexane=7:3→1:0). 4N Hydrochloride-ethyl acetate solution (1 ml) was added to the obtained yellow oil, and the precipitated crystals were collected by filtration, and recrystallized to give the title compound (306 mg).

1. filtrationThe reaction solution was filtered through celite
2. customThe solvent was evaporated under reduced pressure
3. customThe residue was purified by basic silica gel column chromatography (ethyl acetate:hexane=7:3→1:0)
4. addition4N Hydrochloride-ethyl acetate solution (1 ml) was added to the obtained yellow oil
5. filtrationthe precipitated crystals were collected by filtration
6. customrecrystallized