反应详情

温度

70 °C

A mixture of 2,2,2-trichloroethyl (3,4-dimethylisoxazol-5-yl)carbamate (277 mg, 0.964 mmol), 3-(2-piperazin-1-yl-1,3-thiazol-4-yl)benzonitrile (237 mg, 0.877 mmol) and diisopropylethylamine (0.305 ml, 1.75 mmol) in dimethyl sulfoxide (2.9 ml) was stirred at 70° C. for 15 hours. Water was poured to the reaction mixture, 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 (hexane:ethyl acetate=1:1), and recrystallized from a mixed solvent of hexane and ethyl acetate to give 142 mg (39.6%) 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 (hexane:ethyl acetate=1:1)
6. customrecrystallized from a mixed solvent of hexane and ethyl acetate