反应详情

A 50 mL round-bottomed flask was charged with 4-chloro-3-nitrobenzenesulfonamide (1 g, 4.23 mmol), 4-methylpiperazin-1-amine dihydrochloride (1 g, 5.32 mmol), and N1,N1,N2,N2-tetramethylethane-1,2-diamine (3 mL, 20.01 mmol) in dioxane (10 mL). The reaction mixture was refluxed for 12 hours. After this time, the reaction mixture was cooled to room temperature, the salt filtered off via a Buchner funnel, and the solvent removed in vacuo. The crude product was added to a silica gel column (Analogix, SF65-200 g) and purified by eluting with 0-5% methanol in dichloromethane.

1. temperatureThe reaction mixture was refluxed for 12 hours
2. filtrationthe salt filtered off via a Buchner funnel
3. customthe solvent removed in vacuo
4. additionThe crude product was added to a silica gel column (Analogix
5. customSF65-200 g) and purified
6. washby eluting with 0-5% methanol in dichloromethane