反应详情

5.00 g (28.1 mmoles) of 2,5-dichlorophenoxyamine was dissolved in 6.8 ml of pyridine, and then 3.02 g (28.1 mmoles) of dimethylcarbamoyl chloride was added. The mixture was stirred at a temperature of from 25° to 30° C. for 12 hours. After an addition of 200 ml of water, the reaction mixture was extracted with ethyl acetate. The extract was washed with a saturated sodium chloride aqueous solution, and dried over anhydrous magnesium sulfate. Ethyl acetate was distilled off under reduced pressure, and precipitated crystals were washed with hexane, whereby 4.33 g of the desired product was obtained as light yellow crystals (yield: 62%).

1. extractionthe reaction mixture was extracted with ethyl acetate
2. washThe extract was washed with a saturated sodium chloride aqueous solution
3. dry with materialdried over anhydrous magnesium sulfate
4. distillationEthyl acetate was distilled off under reduced pressure
5. customprecipitated crystals
6. washwere washed with hexane