3-溴-2-(二氟甲氧基)苯胺

反应条件: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 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%). Into a 300-ml four-necked flask provided with a reflux condenser, a stirrer Thereto was slowly added, at 80 to 85° C. The temperature was increased refluxing with heating After completion of the reaction, azeotropic distillation 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 subjected to distillation to remove the solvent

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Into a 100-ml four-necked flask provided with a reflux condenser, a stirrer and a thermometer were fed 0.95 g (17.0 mmol) of an iron powder, 0.11 g (1.0 mmol) of 98% sulfuric acid, 15 ml of water and 1.62 g (6.0 mmol) of 3-bromo-2-difluoromethoxynitrobenzene. The mixture was heated on an oil bath and refluxed for 2 hours. After the completion of a reaction, azeotropic distillation was conducted while 220 ml of water was added gradually. The distillate was subjected to extraction two times each using 100 ml of ether. The ether layer was dried over anhydrous sodium sulfate and then subjected to distillation. The residue was distilled under vacuum to obtain 0.94 g of 3-bromo-2-difluoromethoxyaniline (yield: 65.4%, purity: 98.5%). Into a 100-ml four-necked flask provided with a reflux condenser, a stirrer The mixture was heated on an oil bath refluxed for 2 hours After the completion of a reaction, azeotropic distillation was added gradually The distillate was subjected to extraction two times each using 100 ml of ether The ether layer was dried over anhydrous sodium sulfate subjected to distillation The residue was distilled under vacuum

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Into a 100-ml four-necked flask provided with a reflux condenser, a stirrer and a thermometer were fed 0.95 g (17.0 mmol) of an iron powder, 0.11 g (1.0 mmol) of 98% sulfuric acid, 15 ml of water and 1.62 g (6.0 mmol) of 3-bromo-2-difluoromethoxynitrobenzene. The mixture was heated on an oil bath and refluxed for 2 hours. After the completion of a reaction, azeotropic distillation was conducted while 220 ml of water was added gradually. The distillate was subjected to extraction two times each using 100 ml of ether. The ether layer was dried over anhydrous sodium sulfate and then subjected to distillation. The residue was distilled under vacuum to obtain 0.94 g of 3-bromo-2-difluoromethoxyaniline (yield: 65.4%, purity: 98.5%). Into a 100-ml four-necked flask provided with a reflux condenser, a stirrer The mixture was heated on an oil bath refluxed for 2 hours After the completion of a reaction, azeotropic distillation was added gradually The distillate was subjected to extraction two times each using 100 ml of ether The ether layer was dried over anhydrous sodium sulfate subjected to distillation The residue was distilled under vacuum

反应条件: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 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%). Into a 300-ml four-necked flask provided with a reflux condenser, a stirrer Thereto was slowly added, at 80 to 85° C. The temperature was increased refluxing with heating After completion of the reaction, azeotropic distillation 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 subjected to distillation to remove the solvent

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Into a 100-ml four-necked flask provided with a reflux condenser, a stirrer and a thermometer were fed 0.95 g (17.0 mmol) of an iron powder, 0.11 g (1.0 mmol) of 98% sulfuric acid, 15 ml of water and 1.62 g (6.0 mmol) of 3-bromo-2-difluoromethoxynitrobenzene. The mixture was heated on an oil bath and refluxed for 2 hours. After the completion of a reaction, azeotropic distillation was conducted while 220 ml of water was added gradually. The distillate was subjected to extraction two times each using 100 ml of ether. The ether layer was dried over anhydrous sodium sulfate and then subjected to distillation. The residue was distilled under vacuum to obtain 0.94 g of 3-bromo-2-difluoromethoxyaniline (yield: 65.4%, purity: 98.5%). Into a 100-ml four-necked flask provided with a reflux condenser, a stirrer The mixture was heated on an oil bath refluxed for 2 hours After the completion of a reaction, azeotropic distillation was added gradually The distillate was subjected to extraction two times each using 100 ml of ether The ether layer was dried over anhydrous sodium sulfate subjected to distillation The residue was distilled under vacuum