Reaktion #74864

ord-29ec567dce774185bea2d359c3e4c5f8

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONA mixture of 2.0 g
  2. 2
    Temperaturunder reflux for 6 hours
  3. 3
    TemperaturThe mixture was cooled
  4. 4
    Sonstigethe benzene was removed in vacuo
  5. 5
    Sonstigethe column was flushed with benzene
  6. 6
    SonstigeThe product was then removed from the column with denatured ethanol
  7. 7
    SonstigeThe ethanol was removed
  8. 8
    Sonstigethe 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°.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04174209uspto-grants-1979_11