反应详情

A mixture of 3-(trifluoromethyl)-4-nitroaniline (1.00 g, 4.85 mmol) and benzoyl chloride (0.62 ml, 5.34 mmol) were heated in pyridine (20 ml) at reflux for 3 hours under an inert atmosphere. The reaction was allowed to cool to ambient temperature, poured into water (200 ml) and basified by addition of 2.0 N aqueous sodium hydroxide solution. An oily liquid separated out which crystallised on standing at 4° C. overnight. The solid was collected by suction filtration, washed with water (3×20 ml) and then purified by flash chromatography on silica gel, eluting with dichloromethane. This yielded N-benzoyl 3-(trifluoromethyl)-4-nitroaniline (1.01 g, 67% yield) as a white solid:

1. temperatureat reflux for 3 hours under an inert atmosphere
2. customAn oily liquid separated out which
3. customcrystallised
4. filtrationThe solid was collected by suction filtration
5. washwashed with water (3×20 ml)
6. custompurified by flash chromatography on silica gel
7. washeluting with dichloromethane