反应详情

温度

80 °C

Into a 300-ml four-necked flask provided with a reflux condenser, a stirrer and a thermometer were fed 6.56 g of an iron powder, 0.49 g (4.7 mmol) of 95% sulfuric acid and 50 ml of water. The mixture was heated to 80° C. on an oil bath. Thereto was slowly added, at 80 to 85° C., 12.54 g (0.047 mol) of 3-bromo-2-difluoromethoxynitrobenzene. The temperature was increased and refluxing was conducted at 100° C. for 2 hours with heating. After completion of the reaction, azeotropic distillation was performed while 200 ml of water was added gradually. The distillate was subjected to extraction two times each using 30 ml of dichloromethane. The organic layer was dried over anhydrous sodium sulfate and subjected to distillation to remove the solvent and obtain 8.09 g of 3-bromo-2-difluoromethoxyaniline (yield: 72.4%, purity: 99.7%).

1. customInto a 300-ml four-necked flask provided with a reflux condenser, a stirrer
2. additionThereto was slowly added, at 80 to 85° C.
3. temperatureThe temperature was increased
4. temperaturerefluxing
5. temperaturewith heating
6. customAfter completion of the reaction, azeotropic distillation
7. additionwas added gradually
8. extractionThe distillate was subjected to extraction two times each using 30 ml of dichloromethane
9. dry with materialThe organic layer was dried over anhydrous sodium sulfate
10. distillationsubjected to distillation
11. customto remove the solvent