反应详情

4.5 g (25 mmol) of 2,5-dichlorophenoxyamine was dissolved in 10 ml of pyridine, and then 5.6 g (38 mmol) of methoxymethylcarbamoyl 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, and precipitated crystals were recrystallized from ethyl acetate-hexane, whereby 4.8 g of the desired product was obtained (yield: 72%).

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
5. customprecipitated crystals
6. customwere recrystallized from ethyl acetate-hexane