反应详情

Into a 200-ml four-necked flask provided with a reflux condenser, a thermometer and a stirrer were fed 7.96 g (0.05 mol) of 3,4-difluoro-2-methoxyaniline, 40 g (0.67 mol) of acetic acid and 100 ml of ethanol. To the resulting mixture being stirred at room temperature was dropwise added 9.24 g (0.053 mol) of 1-ethoxy-1-trimethylsilyloxycyclopropane. The resulting mixture was placed on an oil bath and refluxed at 80° C. for 3 hours with stirring, in a nitrogen current. The resulting reaction mixture was concentrated under aspirator vacuum by the use of a rotary evaporator. Lastly, the acetic acid remaining in the resulting residue was removed by the use of a vacuum pump to obtain 11.5 g of an oily substance. This oily substance was subjected to vacuum distillation to obtain 10.1 g (yield: 83.0%) of N-(1-ethoxy)cyclopropyl-3,4-difluoro-2-methoxyaniline.

1. customInto a 200-ml four-necked flask provided with a reflux condenser
2. customThe resulting mixture was placed on an oil bath
3. temperaturerefluxed at 80° C. for 3 hours
4. stirringwith stirring, in a nitrogen current
5. customThe resulting reaction mixture
6. concentrationwas concentrated under aspirator vacuum by the use of a rotary evaporator
7. customLastly, the acetic acid remaining in the resulting residue was removed by the use of a vacuum pump
8. customto obtain 11.5 g of an oily substance
9. distillationThis oily substance was subjected to vacuum distillation