反应详情

A mixture of 3-cyanamidobenzotrifluoride (0.40 g, 2.15 mmol), 2-methoxy-5-triflouromethylaniline hydrochloric acid salt (0.53 g, 2.33 mmol) and acetonitrile (20 ml) was stirred at reflux for 40 h. The solvent was evaporated. Dichloromethane (50 ml) was added and the mixture was washed with saturated aqueous sodium hydrogen carbonate (50 ml). The organic phase was purified by chromatography using silica gel and a mixture of methanol (10%) and dichloromethane as eluent. The product was isolated as the free base. Yield 0.40 g, 49%. M.p. 45-47° C.

1. temperatureat reflux for 40 h
2. customThe solvent was evaporated
3. additionDichloromethane (50 ml) was added
4. washthe mixture was washed with saturated aqueous sodium hydrogen carbonate (50 ml)
5. customThe organic phase was purified by chromatography
6. additiona mixture of methanol (10%) and dichloromethane as eluent
7. customThe product was isolated as the free base