反应详情

A mixture of 2-nitro-4-trifluoromethylbenzonitrile (8.64 g), thiophenol (4.4 g) and potassium carbonate (6.9 g) in acetonitrile was stirred at room temperature for 1 hour then heated at reflux for 9 hours. Thiophenol (0.3 ml) was added and the mixture was stirred and heated at reflux for 1 hour. Water was added and the mixture was extracted with dichloromethane, dried (MgSO4) and filtered. The flitrate was evaporated to dryness and the residue was recrystallized from n-hexane to give 2-(phenylsulphenyl)-4-trifluoromethylbenzonitrile (9.5 g) as a white solid, m.p. 51° C.

1. temperaturethen heated
2. temperatureat reflux for 9 hours
3. stirringthe mixture was stirred
4. temperatureheated
5. temperatureat reflux for 1 hour
6. extractionthe mixture was extracted with dichloromethane
7. dry with materialdried (MgSO4)
8. filtrationfiltered
9. customThe flitrate was evaporated to dryness
10. customthe residue was recrystallized from n-hexane