反应详情

温度

80 °C

A mixture of 1-(6-chloronaphthalene-2-sulfonyl)-4-(6-chloropyridazin-3-ylcarbonyl)piperazine (0.2 g, 0.443 mmol), 1-methylhexahydro-1,4-diazepine (0.166 mL, 1.33 mmol) and pyridine (0.11 mL, 1.33 mmol) in DMSO (5 mL) was heated in a sealed tube at 80° C. overnight. The reaction mixture was cooled to room temperature, diluted with ethyl acetate (500 mL), washed with saturated sodium bicarbonate (200 mL), water (2×150 mL) and brine, and dried over sodium sulfate. After filtration and evaporation of the solvent, the residue was purified by flash chromatography over silica, eluting with 5–7% methanol/methylene chloride, to afford the title compound (0.1 g, 43%).

1. temperatureThe reaction mixture was cooled to room temperature
2. washwashed with saturated sodium bicarbonate (200 mL), water (2×150 mL) and brine
3. dry with materialdried over sodium sulfate
4. filtrationAfter filtration and evaporation of the solvent
5. customthe residue was purified by flash chromatography over silica
6. washeluting with 5–7% methanol/methylene chloride