反应详情

温度

70 °C

A mixture of bis(2,2,2-trichloroethyl) imidazo[1,2-b]pyridazin-6-ylimidodicarbonate (295 mg, 0.609 mmol), 1-(3-phenyl-1,2,4-thiadiazol-5-yl)piperazine (300 mg, 1.22 mmol) and diisopropylethylamine (0.106 ml, 0.609 mmol) in dimethylsulfoxide (2.0 ml) was stirred at 70° C. for 4 hours. Water was poured into the reaction solution, and the mixture was extracted with ethyl acetate. The extract was washed with water and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate) and recrystallized from a mixed solvent of hexane and tetrahydrofuran to give 212 mg (85.7%) of the desired product as a solid.

1. extractionthe mixture was extracted with ethyl acetate
2. washThe extract was washed with water
3. dry with materialdried over anhydrous magnesium sulfate
4. distillationthe solvent was distilled off under reduced pressure
5. customThe residue was purified by silica gel column chromatography (ethyl acetate)
6. customrecrystallized from a mixed solvent of hexane and tetrahydrofuran