反应详情

N-[4-(2,4-Dioxo-1,2,3,4,8,9,10,11-octahydronaphtho[1,2-b][1,4]diazepine-5-yl)phenyl]-N-methyl-2-nitrobenzenesulfonamide (50 mg, 0.096 mmol) was dissolved in dry dimethylformamide (2 mL). To the solution were added potassium carbonate (40 mg, 0.29 mmol), and then thiophenol (12 μL, 0.12 mmol). The mixture was stirred overnight at room temperature. To the reaction mixture was added cold water. The mixture was extracted with ethyl acetate, washed with saturated brine, and dried over anhydrous sodium sulfate. The solvent was removed by evaporation under reduced pressure. The residue was purified by silica gel column chromatography (chloroform) to give 5-(4-methylaminophenyl)-1,5,8,9,10,11-hexahydronaphtho[1,2-b][1,4]diazepine-2,4-dione as a colorless amorphous form (32 mg, 0.095 mmol).

1. extractionThe mixture was extracted with ethyl acetate
2. washwashed with saturated brine
3. dry with materialdried over anhydrous sodium sulfate
4. customThe solvent was removed by evaporation under reduced pressure
5. customThe residue was purified by silica gel column chromatography (chloroform)