Reaktion #74864
ord-29ec567dce774185bea2d359c3e4c5f8
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1workup.ADDITIONA mixture of 2.0 g
- 2Temperaturunder reflux for 6 hours
- 3TemperaturThe mixture was cooled
- 4Sonstigethe benzene was removed in vacuo
- 5Sonstigethe column was flushed with benzene
- 6SonstigeThe product was then removed from the column with denatured ethanol
- 7SonstigeThe ethanol was removed
- 8Sonstigethe residue was crystallized from ether yielding 0.7 g
Vorschrift
A mixture of 2.0 g. of 1-methyl-3-phenyl-5-(3-trifluoromethylphenyl)-4(1H)-pyridinethione and 10 ml. of benzyl chloride in benzene was heated under reflux for 6 hours. The mixture was cooled and the benzene was removed in vacuo. The residue was put on a silica gel column in benzene and the column was flushed with benzene. The product was then removed from the column with denatured ethanol. The ethanol was removed and the residue was crystallized from ether yielding 0.7 g. of 4-benzylthio-1-methyl-3-phenyl-5-(3-trifluoromethylphenyl)pyridinium chloride, m.p. 70°-73°.