反应详情

温度

70 °C

A mixture of 2,2,2-trichloroethyl (4-bromo-1-methyl-1H-pyrazol-5-yl)carbamate (289 mg, 0.822 mmol), 1-(3-phenyl-1,2,4-thiadiazol-5-yl)piperazine (184 mg, 0.747 mmol) and diisopropylethylamine (0.143 ml, 0.822 mmol) in dimethylsulfoxide (2.5 ml) was stirred at 70° C. for 15.5 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 recrystallized from a mixed solvent of hexane and tetrahydrofuran to give 233 mg (69.7%) 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 recrystallized from a mixed solvent of hexane and tetrahydrofuran