反应详情

2-Amino-4-trifluoromethylthiophenol (5.74 g, 25 mmol) was added to a mixture of sodium hydride (2.0 g of 60% oil dispersion, 50 mmol) in DMF (100 ml) at 0° under nitrogen. After stirring for 30 minutes at 0°, 2-fluoro-3-trifluoromethylbenzonitrile (4.73 g, 25 mmol) in DMF (20 ml) was added and the mixture kept at room temperature overnight. The reaction mixture was evaporated and azeotroped with toluene, then the residue was partitioned between chloroform and water and the layers separated. Drying (magnesium sulphate) and evaporation of the organic layer gave a residue which was purified by chromatography on silica gel, eluting with dichloromethane. Recrystallisation from cyclohexane afforded the product as colourless needles (6.44 g).

1. waitthe mixture kept at room temperature overnight
2. customThe reaction mixture was evaporated
3. customazeotroped with toluene
4. customthe residue was partitioned between chloroform and water
5. customthe layers separated
6. customDrying
7. custom(magnesium sulphate) and evaporation of the organic layer
8. customgave a residue which
9. customwas purified by chromatography on silica gel
10. washeluting with dichloromethane
11. customRecrystallisation from cyclohexane