反应详情

To acetonitrile solution (500 ml) of 3,4,5-trifluoro-benzonitrile (15.0 g, 95.5 mmol), N-ethyldiisopropylamine (33.3 ml, 191 mmol) and 4-methoxy-benzylamine (24.9 ml, 191 mmol) were added, followed by refluxing for 21 hours. The solvent was distilled off under reduced pressure, followed by dissolution in ethyl acetate (500 ml), which was washed with saturated aqueous sodium chloride solution (200 ml). After the organic layer was dried over sodium sulfate, the solvent was distilled off under reduced pressure. This was purified by silica gel column chromatography (dichloromethane), to obtain the desired compound (26.2 g, quant.).

1. temperatureby refluxing for 21 hours
2. distillationThe solvent was distilled off under reduced pressure
3. dissolutionfollowed by dissolution in ethyl acetate (500 ml)
4. washwhich was washed with saturated aqueous sodium chloride solution (200 ml)
5. dry with materialAfter the organic layer was dried over sodium sulfate
6. distillationthe solvent was distilled off under reduced pressure
7. customThis was purified by silica gel column chromatography (dichloromethane)